Composition of matter tailoring: system I

ABSTRACT

The present invention relates to new compositions of matter, particularly metals and alloys, and methods of making such compositions. The new compositions of matter exhibit long-range ordering and unique electronic character.

RELATED APPLICATION

[0001] This application is a divisional of U.S. Ser. No. 10/123,028,filed Apr. 12, 2002, which is a continuation-in-part of U.S. Ser. No.09/416,720, filed Oct. 13, 1999, now U.S. Pat. No. 6,572,792, issuedJun. 3, 2003, and a continuation-in-part of International ApplicationNo. PCT/US00/28549, which designated the United States and was filed onOct. 13, 2000, published in English, which is a continuation of U.S.Ser. No. 09/416,720, filed Oct. 13, 1999. The entire teachings of theabove applications are incorporated herein by reference.

BACKGROUND OF THE INVENTION

[0002] All matter has structure. The structure of matter emanates fromthe electronic structure of the elements of the periodic table. It isthe electronic structure of the elements and the new electronicstructures that arise as a consequence of their combination in moleculesthat define the electronic state and character of matter. It is also theelectronic structure that creates the properties identified andassociated with elements and the matter that results from theircombination and arrangement (e.g., molecules and matter).

[0003] Certain combinations of elements give rise to states of matterwith particularly desirable properties. For instance, certain states ofmatter have long-range order, which refers to matter that has repeatingaligned chemical, electronic, or structural units. Example of suchstates of matter include surfactant membranes, crystals such as smecticliquid crystals and liquid crystalline polymers, and magnetic materials.

[0004] One means of imparting unique properties to a material involvesadding carbon to the material. Depending on the parent material and onthe amount of carbon added, carbon may remain dissolved in a material ormay precipitate out to form discrete carbon structures.

SUMMARY OF THE INVENTION

[0005] The present invention relates to a new composition of mattercomprised of ‘p’, ‘d’, and/or ‘f’ atomic orbitals, and a process formaking the composition of matter. This new composition of matter can bedistinguished by a change in energy, electronic properties, physicalproperties, and the like. X-ray fluorescence spectroscopy is a preferredmethod of detecting and distinguishing new compositions of matter. Thechange in properties can be controlled to be transient, fixed, oradjustable (temporarily permanent) and includes properties such asmechanical, electrical, chemical, thermal, engineering, and physicalproperties, as well structural character of the composition of matter(e.g., alignment, orientation, order, anisotropy, and the like).

[0006] The present invention includes manufactured metals and alloyscharacterized by the x-ray fluorescence spectrometry plots and elementalabundance tables (obtained from x-ray fluorescence analysis) containedherein.

[0007] The present invention is additionally a method of processing ametal or an alloy of metals, comprising the steps of:

[0008] (A.) adding the metal or alloy to a reactor in one or more stepsand melting said metal or alloy;

[0009] (B.) adding a carbon source to the molten metal or alloy anddissolving carbon in said molten metal or alloy, followed by removingthe undissolved carbon source;

[0010] (C.) increasing the temperature of the molten metal or alloy;

[0011] (D.) varying the temperature of the molten metal or alloy betweentwo temperatures over one or more cycles;

[0012] (E.) adding a flow of an inert gas through the molten metal oralloy;

[0013] (F.) varying the temperature of the molten metal or alloy betweentwo temperatures over one or more cycles;

[0014] (G.) adding a carbon source to the molten metal or alloy andfurther dissolving carbon in said molten metal or alloy, followed byremoving the undissolved carbon source;

[0015] (H.) varying the temperature of the molten metal or alloy betweentwo temperatures over one or more cycles, wherein the molten metal oralloy has a greater degree of saturation with carbon than in Step (F.);

[0016] (I.) stopping the flow of the inert gas;

[0017] (J.) varying the temperature of the molten metal or alloy betweentwo temperatures over one or more cycles, wherein the molten metal oralloy has a greater degree of saturation with carbon than in Step (H.)and wherein an inert gas is added as the temperature is lowered and aninert gas, chosen independently, is added as the temperature is raised;

[0018] (K.) varying the temperature of the molten metal or alloy betweentwo temperatures over one or more cycles, wherein the molten metal oralloy has a greater degree of saturation with carbon than in Step (J.)and wherein an inert gas is added as the temperature is lowered and aninert gas, chosen independently, is added as the temperature is raised;

[0019] (L.) stopping the flow of the inert gases;

[0020] (M.) varying the temperature of the molten metal or alloy betweentwo temperatures over one or more cycles, wherein the molten metal oralloy has an equal or greater degree of saturation with carbon than inStep (K.); and

[0021] (N.) cooling the molten metal or alloy to room temperature,thereby obtaining a solidified manufactured metal or alloy.

[0022] Steps (D.), (F.), (H.), (J.), (K.), and (L.) of the presentmethod are commonly referred to as “cycling steps” below. For purposesof the present invention, carbon “dissolved” in a metal is defined ascarbon that has been solubilized in a molten metal, adsorbed by a metal,reacted with a metal, or has otherwise interacted with a metal such thatcarbon is desorbed or transferred from a solid carbon source into amolten metal.

[0023] Preferably, the present invention is a method of processingcopper, comprised of the steps described above.

[0024] The present invention also includes a method of processing ametal or an alloy of metals, comprising the steps of:

[0025] (A.) adding the metal or alloy to a reactor in one or more stepsand melting said metal or alloy;

[0026] (B.) adding a carbon source to the molten metal or alloy anddissolving carbon in said molten metal or alloy, followed by removingthe undissolved carbon source;

[0027] (C.) varying the temperature of the molten metal or alloy betweentwo temperatures over two or more cycles;

[0028] (D.) adding a carbon source to the molten metal or alloy andfurther dissolving carbon in said molten metal or alloy, followed byremoving the undissolved carbon source;

[0029] (E.) varying the temperature of the molten metal or alloy betweentwo temperatures over two or more cycles, wherein the molten metal oralloy has a greater degree of saturation with carbon than in Step (D.);and

[0030] (F.) cooling the molten metal or alloy to room temperature,thereby obtaining a solidified manufactured metal or alloy;

[0031] further characterized by adding a flow of inert gas, before,during, or after one or more of Steps (B.) through (E.).

[0032] In another embodiment, the present invention is a method ofprocessing copper, or other metal or alloy comprising:

[0033] (1) contacting molten copper or other metal or alloy with acarbon source;

[0034] (2.) an iterative cycling process, wherein relative saturation ofcopper or other metal or alloy with carbon remains the same or increasesindependently with each cycle; and

[0035] (3.) cooling the molten copper or other metal or alloy to roomtemperature, thereby obtaining a solidified manufactured copper or othermetal or alloy.

[0036] Advantages of the present invention include a method ofprocessing metals into new compositions of matter and producing andcharacterizing compositions of matter with altered physical and/orelectrical properties.

BRIEF DESCRIPTION OF THE DRAWINGS

[0037]FIGS. 1A and 1B show non-contact magnetic force microscopy imagesof natural copper and manufactured copper, respectively.

[0038]FIG. 2A shows non-contact magnetic force microscopy ofmanufactured copper.

[0039]FIG. 2B shows scanning tunneling microscopy images of manufacturedcopper.

[0040]FIGS. 3A, 3B, and 4A and 4B show x-ray emission spectrometryimages of natural copper and manufactured copper.

[0041]FIG. 5A shows a non-contact magnetic force microscopy image ofmanufactured copper. FIG. 5B shows a x-ray emission spectroscopy imageof manufactured copper.

[0042]FIGS. 6A and 6B show a plot of an x-ray fluorescence spectrometrycomparison of manufactured copper and natural copper.

[0043]FIG. 7 shows a plot of an X-ray fluorescence spectrometry inrelation to the direction of the scan.

[0044]FIG. 8 shows a plot of a change in capacitance and voltage decayfor a manufactured metal.

[0045]FIG. 9 shows a plot of a change in voltage gradients for a moltenmanufactured metal as the position of an electrode within the melt ischanged.

[0046]FIG. 10 shows a plot of the observed voltage of a manufacturedcopper-nickel alloy, as measured in a molten state.

[0047]FIG. 11 shows a plot of the observed voltage of a manufacturedmetal, as measured in a molten state.

[0048]FIG. 12 shows a plot of a positive voltage signature and positivecapacitance decay of a manufactured metal, as measured in a moltenstate.

[0049]FIG. 13 shows a plot of a voltage decay profile of a manufacturedmetal, as measured in a molten state.

[0050]FIG. 14 shows a plot of a neutral decay in voltage andcapacitance, as measured in a molten state.

[0051]FIG. 15 shows a plot of a positive voltage signature and anegative capacitance decay of a manufactured metal, as measured in amolten state.

[0052]FIG. 16 shows a plot of the voltage over time of a manufacturedmetal under pressure.

[0053]FIGS. 17A, 17B, 17C, 18A, 18B and 18C show optical and scanningelectron microscopy images of manufactured copper.

[0054]FIGS. 19A, 19B, 20A and 20B show optical microscopy images ofmanufactured nickel.

[0055]FIGS. 21A, 21B and 21C show images of atomic force microscopy andscanning tunneling microscopy of manufactured copper from an axialanalysis.

[0056]FIGS. 22A, 22B and 22C show images of atomic force microscopy andnon-contact magnetic force microscopy of manufactured copper from aradial analysis.

[0057]FIGS. 23A, 23B and 23C show images of discrete induced magnetismof non-magnetic copper.

[0058]FIG. 24 shows a plot of electrical susceptance for manufacturedcompositions in comparison to the compositions in its natural state.

[0059]FIG. 25 shows a plot of x-ray fluorescence spectrometry formanufactured copper, on both the axial and radial faces of a block cutfrom the ingot prepared in Example 1, as compared to a plot of x-rayfluorescence spectrometry for natural copper.

[0060]FIG. 26 shows a plot of x-ray fluorescence spectrometry formanufactured copper in the region of the K_(α) band of aluminum, on thebottom face of a block cut from the ingot prepared in Example 1, ascompared to a plot of x-ray fluorescence spectrometry for naturalaluminum.

[0061]FIGS. 27A and 27B show plots of x-ray fluorescence spectrometryfor manufactured nickel, on both the axial and radial faces of a blockcut from the ingot prepared in Example 2, as compared to plots of x-rayfluorescence spectrometry for natural nickel.

[0062]FIG. 28A shows a plot of x-ray fluorescence spectrometry formanufactured nickel in the region of the K_(α) band of aluminum, on theaxial and radial faces of a block cut from the ingot prepared in Example2, as compared to a plot of x-ray fluorescence spectrometry for naturalaluminum.

[0063]FIG. 28B shows a plot of x-ray fluorescence spectrometry formanufactured nickel in the region of the K_(α) band of zirconium, on theaxial and radial faces of a block cut from the ingot prepared in Example2, as compared to a plot of x-ray fluorescence spectrometry for naturalzirconium.

[0064]FIG. 29 shows a plot of x-ray fluorescence spectrometry formanufactured nickel in the region of the K_(α) band of sulfur, on allsix faces of a block cut from the ingot prepared in Example 2, ascompared to a plot of x-ray fluorescence spectromertry for naturalsulfur.

[0065]FIG. 30 shows a plot of x-ray fluorescence spectrometry formanufactured nickel in the region of the K_(α) band of chlorine (frompotassium chloride), on the axial and radial faces of a block cut fromthe ingot prepared in Example 2, as compared to a plot of x-rayfluorescence spectrometry for natural chlorine (from potassiumchloride).

[0066]FIGS. 31A and 31B show plots of x-ray fluorescence spectrometryfor manufactured cobalt, on both the axial and radial faces of a blockcut from the ingot prepared in Example 3, as compared to plots of x-rayfluorescence spectrometry for natural cobalt.

[0067]FIGS. 32A shows a plot of x-ray fluorescence spectrometry formanufactured cobalt in the region of the K_(α) band of aluminum, on theaxial and radial faces of a block cut from the ingot prepared in Example3, as compared to a plot of x-ray fluorescence spectrometry for naturalaluminum.

[0068]FIG. 32B shows a plot of x-ray fluorescence spectrometry formanufactured cobalt in the region of the K_(α) band of iron, on theaxial and radial faces of a block cut from the ingot prepared in Example3, as compared to a plot of x-ray fluorescence spectrometry for naturaliron.

[0069]FIG. 33A shows a plot of x-ray fluorescence spectrometry formanufactured cobalt in the region of the K_(α) band of chlorine (frompotassium chloride), on the axial and radial faces of a block cut fromthe ingot prepared in Example 3, as compared to a plot of x-rayfluorescence spectrometry for natural chlorine (from potassiumchloride).

[0070]FIG. 33B shows a plot of x-ray fluorescence spectrometry formanufactured cobalt in the region of the K_(α) band of zirconium, on theaxial and radial faces of a block cut from the ingot prepared in Example3, as compared to a plot of x-ray fluorescence spectrometry for naturalzirconium.

[0071]FIG. 34 shows a plot of x-ray fluorescence spectrometry formanufactured cobalt in the region of the K_(α) band of manganese, on theaxial and radial faces of a block cut from the ingot prepared in Example3, as compared to a plot of x-ray fluorescence spectrometry for naturalmanganese.

[0072]FIG. 35 shows a plot of x-ray fluorescence spectrometry for amanufactured copper/silver/gold alloy in the region of the K_(α) band ofcopper, on the axial and radial faces of a block cut from the ingotprepared in Example 4, as compared to a plot of x-ray fluorescencespectrometry for natural copper.

[0073]FIG. 36 shows a plot of x-ray fluorescence spectrometry for amanufactured copper/silver/gold alloy in the region of the K_(α) band ofgold, on the axial and radial faces of a block cut from the ingotprepared in Example 4, as compared to a plot of x-ray fluorescencespectrometry for natural silver.

[0074]FIG. 37 shows a plot of x-ray fluorescence spectrometry for amanufactured copper/silver/gold alloy in the region of the K_(α) band ofsilver, on the axial and radial faces of a block cut from the ingotprepared in Example 4, as compared to a plot of x-ray fluorescencespectrometry for natural gold.

[0075]FIG. 38 shows a plot of x-ray fluorescence spectrometry for amanufactured tin/lead/zinc alloy in the region of the K_(α) band of tin,on the axial and radial faces of a block cut from the ingot prepared inExample 5, as compared to a plot of x-ray fluorescence spectrometry fornatural tin.

[0076]FIG. 39 shows a plot of x-ray fluorescence spectrometry for amanufactured tin/lead/zinc alloy in the region of the K_(α) band ofzinc, on the axial and radial faces of a block cut from the ingotprepared in Example 5, as compared to a plot of x-ray fluorescencespectrometry for natural zinc.

[0077]FIG. 40 shows a plot of x-ray fluorescence spectrometry for amanufactured tin/lead/zinc alloy in the region of the K_(α) band oflead, on the axial and radial faces of a block cut from the ingotprepared in Example 5, as compared to a plot of x-ray fluorescencespectrometry for natural lead.

[0078]FIG. 41 shows a plot of x-ray fluorescence spectrometry for amanufactured tin/sodium/magnesium/potassium alloy in the region of theK_(α) band of potassium (from potassium chloride), on the axial andradial faces of a block cut from the ingot prepared in Example 6, ascompared to a plot of x-ray fluorescence spectrometry for naturalpotassium (from potassium chloride).

[0079]FIG. 42 shows a plot of x-ray fluorescence spectrometry for amanufactured tin/sodium/magnesium/potassium alloy in the region of theK_(α) band of tin, on the axial and radial faces of a block cut from theingot prepared in Example 6, as compared to a plot of x-ray fluorescencespectrometry for natural tin.

[0080]FIG. 43 shows a plot of x-ray fluorescence spectrometry for amanufactured tin/sodium/magnesium/potassium alloy in the region of theK_(α) band of magnesium (using magnesium oxide), on the axial and radialfaces of a block cut from the ingot prepared in Example 6, as comparedto a plot of x-ray fluorescence spectrometry for natural magnesium(using magnesium oxide).

[0081]FIG. 44 shows a plot of x-ray fluorescence spectrometry for amanufactured tin/sodium/magnesium/potassium alloy in the region of theK_(α) band of sodium (using AlNa₃F₆), on the axial and radial faces of ablock cut from the ingot prepared in Example 6, as compared to a plot ofx-ray fluorescence spectrometry for natural sodium (using AlNa₃F₆).

[0082]FIGS. 45A and 45B show plots of x-ray fluorescence spectrometryfor manufactured silicon, on both the axial and radial faces of a blockcut from the ingot prepared in Example 7, as compared to plots of x-rayfluorescence spectrometry for natural silicon.

[0083]FIG. 46A shows a plot of x-ray fluorescence spectrometry formanufactured silicon in the region of the K_(α) band of aluminum, on theaxial and radial faces of a block cut from the ingot prepared in Example7, as compared to a plot of x-ray fluorescence spectrometry for naturalaluminum.

[0084]FIG. 46B shows a plot of x-ray fluorescence spectrometry formanufactured silicon in the region of the K_(α) band of titanium, on theaxial and radial faces of a block cut from the ingot prepared in Example7, as compared to a plot of x-ray fluorescence spectrometry for naturaltitanium.

[0085]FIG. 47A shows a plot of x-ray fluorescence spectrometry formanufactured silicon in the region of the K_(α) band of sulfur, on theaxial and radial faces of a block cut from the ingot prepared in Example7, as compared to a plot of x-ray fluorescence spectrometry for naturalsulfur.

[0086]FIG. 47B shows a plot of x-ray fluorescence spectrometry formanufactured silicon in the region of the K_(α) band of chlorine (frompotassium chloride), on the axial and radial faces of a block cut fromthe ingot prepared in Example 7, as compared to aplot of x-rayfluorescence spectrometry for natural chlorine (from potassiumchloride).

[0087]FIG. 48A shows a plot of x-ray fluorescence spectrometry formanufactured silicon in the region of the K_(α) band of gallium (fromgallium oxide), on the axial and radial faces of a block cut from theingot prepared in Example 7, as compared to a plot of x-ray fluorescencespectrometry for natural gallium (from gallium oxide).

[0088]FIG. 48B shows a plot of x-ray fluorescence spectrometry formanufactured silicon in the region of the K_(α) band of potassium (frompotassium chloride), on the axial and radial faces of a block cut fromthe ingot prepared in Example 7, as compared to a plot of x-rayfluorescence spectrometry for natural potassium (from potassiumchloride).

[0089]FIGS. 49A and 49B show plots of x-ray fluorescence spectrometryfor manufactured iron, on both the axial and radial faces of a block cutfrom the ingot prepared in Example 8, as compared to plots of x-rayfluorescence spectrometry for natural iron.

[0090]FIG. 50A shows a plot of x-ray fluorescence spectrometry formanufactured iron in the region of the K_(α) band of aluminum, on theaxial and radial faces of a block cut from the ingot prepared in Example8, as compared to a plot of x-ray fluorescence spectrometry for naturalaluminum.

[0091]FIG. 50B shows a plot of x-ray fluorescence spectrometry for 10manufactured iron in the region of the K_(α) band of zirconium, on theaxial and radial faces of a block cut from the ingot prepared in Example8, as compared to a plot of x-ray fluorescence spectrometry for naturalzirconium.

[0092]FIG. 51A shows a plot of x-ray fluorescence spectrometry formanufactured iron in the region of the K_(α) band of sulfur, on theaxial and radial 15 faces of a block cut from the ingot prepared inExample 8, as compared to a plot of x-ray fluorescence spectrometry fornatural sulfur.

[0093]FIG. 51B shows a plot of x-ray fluorescence spectrometry formanufactured iron in the region of the K_(α) band of chlorine (frompotassium chloride), on the axial and radial faces of a block cut fromthe ingot prepared in Example 8, as compared to a plot of x-rayfluorescence spectrometry for natural chlorine (from potassiumchloride).

[0094]FIG. 52 shows a plot of x-ray fluorescence spectrometry for amanufactured iron/vanadium/chromium/manganese alloy in the region of theK_(α) band of chromium (using chromium(m) oxide), on the axial andradial faces of a block cut from the ingot prepared in Example 9, ascompared to a plot of x-ray fluorescence spectrometry for naturalchromium (using chromium (III) oxide).

[0095]FIG. 53 shows a plot of x-ray fluorescence spectrometry for amanufactured iron/vanadium/chromium/manganese alloy in the region of theK_(α) band of iron, on the axial and radial faces of a block cut fromthe ingot prepared in Example 9, as compared to a plot of x-rayfluorescence spectrometry for natural iron.

[0096]FIG. 54 shows a plot of x-ray fluorescence spectrometry for amanufactured iron/vanadium/chromium/manganese alloy in the region of theK_(α) band of vanadium, on the axial and radial faces of a block cutfrom the ingot prepared in Example 9, as compared to a plot of x-rayfluorescence spectrometry for natural vanadium.

[0097]FIG. 55 shows a plot of x-ray fluorescence spectrometry for amanufactured iron/vanadium/chromium/manganese alloy in the region of theK_(α) band of manganese, on the axial and radial faces of a block cutfrom the ingot prepared in Example 9, as compared to a plot of x-rayfluorescence spectrometry for natural manganese.

[0098]FIG. 56 shows a plot of x-ray fluorescence spectrometry for amanufactured iron/vanadium/chromium/manganese alloy in the region of theK_(α) band of sulfur, on all six sides of a block cut from the ingotprepared in Example 9.

[0099]FIG. 57 shows a plot of x-ray fluorescence spectrometry for amanufactured nickel/tantalum/hafnium/tungsten alloy in the region of theK_(α) band of tantalum, on the axial and radial faces of a block cutfrom the ingot prepared in Example 10, as compared to a plot of x-rayfluorescence spectrometry for natural tantalum.

[0100]FIG. 58 shows a plot of x-ray fluorescence spectrometry for amanufactured nickel/tantalum/hafnium/tungsten alloy in the region of theK_(α) band of tungsten, on the axial and radial faces of a block cutfrom the ingot prepared in Example 10, as compared to a plot of x-rayfluorescence spectrometry for natural tungsten.

[0101]FIG. 59 shows a plot of x-ray fluorescence spectrometry for amanufactured nickel/tantalumlhafnium/tungsten alloy in the region of theK_(α) band of hafnium, on the axial and radial faces of a block cut fromthe ingot prepared in Example 10, as compared to a plot of x-rayfluorescence spectrometry for natural hafnium.

[0102]FIG. 60 shows a plot of x-ray fluorescence spectrometry for amanufactured nickelltantalum/hafnium/tungsten alloy in the region of theK_(α) band of sulfur, on all six faces of a block cut from the ingotprepared in Example 10.

[0103]FIG. 61 shows a plot of x-ray fluorescence spectrometry for amanufactured nickel/tantalum/hafnium/tungsten alloy in the region of theK_(α) band of nickel, on the axial and radial faces of a block cut fromthe ingot prepared in Example 10, as compared to a plot of x-rayfluorescence spectrometry for natural nickel.

[0104]FIG. 62 shows the general configuration of the ARL 8410spectrometer.

DETAILED DESCRIPTION OF THE INVENTION

[0105] Electromagnetic chemistry is the science that affects thetransfer and circulation of energy in many forms when induced by changesin electromagnetic energy. The theory of Electrodynamics of MovingBodies (Einstein, 1905) mandates that when the electrodynamic componentsof the material are manipulated, changes in the energy levels within theatomic orbitals must be induced. These changes in the atomic orbitalsare the vehicles by which changes in the (material) properties, such asthe magnitude and/or the orientation, can occur. Alignment of theelectrodynamic component induces effects that may result in significantchanges in the underlying material species: (1) alignment of atoms withthe resulting directionality of physical properties; (2) alignment ofenergy levels and the capability to produce harmonics, may establishphysical properties conducive for energy transfer; (3) alignment of theelectrodynamic component include the opening of pathways for freeelectron flow, and; (4) alignment of electrodynamic field phaseorientation.

[0106] The present invention relates to new compositions of matter,referred to herein as “manufactured” metals or alloys of metals. A“manufactured” metal or alloy is a metal or alloy which exhibits achange in electronic structure, such as that seen in a fluid XRFspectrum. The American Heritage College Dictionary, Third Editiondefines “fluid” as changing or tending to change.

[0107] Metals of the present invention are generally p, d, or f blockmetals. Metals include transition metals such as Group 3 metals (e.g.,scandium, yttrium, lanthanum), Group 4 metals (e.g, titanium, zirconium,hafnium), Group 5 metals (vanadium, niobium, tantalum), Group 6 metals(e.g., chromium, molybdenum, tungsten), Group 7 metals (e.g., manganese,technetium, rhenium), Group 8 metals (e.g., iron, ruthenium, osmium),Group 9 metals (e.g., cobalt, rhodium, iridium), Group 10 metals(nickel, palladium, platinum), Group 11 metals (e.g., copper, silver,gold), and Group 12 metals (e.g., zinc, cadmium, mercury). Metals of thepresent invention also include alkali metals (e.g., lithium, sodium,potassium, rubidium, cesium) and alkaline earth metals (e.g., berylliummagnesium, calcium, strontium, barium). Additional metals includealuminum, gallium, indium, tin, lead, boron, germanium, arsenic,antimony, tellurium, bismuth, and silicon.

[0108] The present invention also includes alloys of metals. Alloys aretypically mixtures of metals. Alloys of the present invention can beformed, for example, by melting together two or more of the metalslisted above. Preferred alloys include those comprised of copper, gold,and silver; tin, zinc, and lead; tin, sodium, magnesium, and potassium;iron, vanadium, chromium, and manganese; and nickel, tantalum, hafnium,and tungsten.

[0109] Carbon sources of the present invention include materials thatare partially, primarily, or totally comprised of carbon. Those carbonsources that are non-organic and comprised partially of carbon areprimarily comprised of one or more metals. Suitable carbon sourcesinclude graphite rods, graphite powder, graphite flakes, fullerenes,diamonds, natural gas, methane, ethane, propane, butane, pentane, castiron, iron comprising carbon, steel comprising carbon, and combinationsthereof. A preferred carbon source is a high purity (<5 ppm impurities)carbon source. Another preferred carbon source is a high purity (<5 ppmimpurities) graphite rod. The carbon source is selected, in part, basedon the system to which it is added. In one example, graphite rods andgraphite flakes are added to copper, typically in a sequential manner.In another example, graphite rods and graphite powder are added to iron,typically in a sequential manner.

[0110] Carbon sources can be contacted with molten metals for variableperiods of time. The period of time the carbon source is in contact withmolten metals is the time between adding the carbon source and removingthe undissolved carbon source. The period of time can be from about 0.5hours to about 12 hours, about 1 hour to about 10 hours, about 2 hoursto about 8 hours, about 3 hours to about 6 hours, about 3.5 hours toabout 4.5 hours, or about 3.9 hours to about 4.1 hours. Alternatively,the period of time can be from about 5 minutes to about 300 minutes,about 10 minutes to about 200 minutes, about 20 minutes to about 120minutes, about 30 minutes to about 90 minutes, about 40 minutes to about80 minutes, about 50 minutes to about 70 minutes, or about 59 minutes toabout 61 minutes.

[0111] A cycle of the present invention includes a period of time wherethe temperature and/or the degree to which a metal is saturated withcarbon is varied. Over a period of time, varying the temperatureinvolves a period of raising (or increasing) the temperature of a metalor alloy and a period when the temperature of a metal or alloy decreases(either passively, such as by heat transfer to the surroundingenvironment, or actively, such as by mechanical means), in any order.Inert gas can be added during a cycle, except where it is specified thatinert gas addition is ceased prior to that cycle. Increasing thetemperature of the metal or alloy increases the amount of carbon thatcan be dissolved into that metal or alloy, which therefore decreases thedegree to which the metal or alloy is saturated with carbon (relative tothe temperature and degree of carbon saturation when graphite saturationassemblies are removed the first time). Similarly, decreasing thetemperature of the metal or alloy increases the (relative) degree towhich the metal or alloy is saturated with carbon.

[0112] The degree to which a metal is saturated with carbon varies overthe course of a method, as well as within each step. In Examples 1-14,the degree of carbon saturation varies between 70% and 95% in the firstcycling step, between 70% and 95% in the second cycling step, between101% and 103% in the third cycling step, between 104% and 107% in thefourth cycling step, between 108% and 118% in the fifth cycling step,and between 114% and 118% in the sixth cycling step. The cycling stepscorrespond to Steps (D.), (F.), (H.), (J.), (K.), and (L.),respectively, of the method described in the third paragraph of thesummary.

[0113] One example of a method of the present invention can be describedin terms of carbon saturation values. After a metal or alloy is added toa suitable reactor, establish the dissolved carbon level at 70% to 95%of the equilibrium saturation of carbon for the thermodynamic statespecified (e.g., T, P, composition) when the composition is in itsnatural state (hereinafter the equilibrium saturation of carbon isreferred to as “[C]_(eqsat)”). Identify temperature set points for 80%and 95% [C]_(eqsat.) Vary the temperature between the predetermined setpoints, such that the temperature is decreased for 7 minutes andincreased over 7 minutes per cycle, for 15 cycles. Next, establish aflow of argon Vary the temperature between the predetermined set points,such that the temperature is decreased for 7 minutes and increased over7 minutes per cycle, for 5 cycles; the temperature should be maintainedabove 70% [C]_(eqsat) at all times and maintained below 95% [C]_(eqsat)at all times. The carbon level is raised to saturation (i.e.,[C]_(eqsal)) with continued argon addition. Hold for 60 minutes atsaturation (i.e., [C]_(eqsat)) with continued argon addition. Raise thecarbon level to ⁺1%_(wt) (i.e., ⁺1%_(wt) represents 1%_(wt) above thesaturation value as defined in its natural state) of [C]_(eqsat) withcontinued argon addition and hold for 5 minutes. Vary the temperaturefor 20 cycles to remain between ⁺1%_(wt) and ⁺3%_(wt) of [C]_(eqsat),such that the temperature is decreased over 9 minutes and increased over9 minutes per cycle. Cease argon addition. Cool the metal to ⁺4%_(wt) of[C]_(eqsat). Vary the temperature for 4.5 cycles to remain between⁺4%_(wt) and ⁺7%_(wt) of [C]_(eqsat), such that the temperature isdecreased over 3 minutes and increased over 5 minutes. Argon is added asthe carbon saturation increases and nitrogen is added as carbonsaturation decreases. Cool the metal to obtain ⁺8%_(wt) with continuedargon addition. Vary the temperature over 15.5 cycles to remain between⁺8%_(wt) and ⁺18%_(wt) of [C]_(eqsat), such that the temperature isdecreased over 15 minutes and increased over 15 minutes. Argon is addedas the carbon saturation increases and nitrogen is added as carbonsaturation decreases. After the 15.5 cycles are complete, gas additionis halted. Perform one complete cycle by varying the temperature toremain between ⁺18%_(wt) to ⁺14%_(wt) of [C]_(eqsat) (ending at⁺18%_(wt)), such that the temperature is increased over 15 minutes anddecreased over 15 minutes. Proceed immediately to a cool down that leadsto solidification.

[0114] An iterative cycle process is a process comprising two or morecycles, whereby one or more of the cycles are carried out at atemperature below the carbon saturation point and one or more cycles arecarried out at a temperature above the carbon saturation point. Forexample, in Example 1, the first cycle is carried out between 2480° F.and 2530° F., the second cycle is carried out between 2480° F. and 2530°F., the third cycle is carried out at 2453° F. and 2459° F., the fourthcycle is carried out between 2441° F. and 2450° F., the fifth cycle iscarried out between 2406° F. and 2438° F., and the sixth cycle iscarried out between 2406° F. and 2419° F. A cycle following an earliercycle can have the identical temperature range as the earlier cycle, apartially overlapping temperature range with the earlier cycle, atemperature range above that of the earlier cycle, or a temperaturecycle below that of the earlier cycle. Partially overlapping temperatureranges includes ranges where one temperature range falls within thelimits of a second temperature range (e.g., 2406° F. to 2438° F. and2406° F. to 2419° F.). Preferably, during an iterative cycling process,the degree to which the metal or alloy is saturated with carbonincreases over the process.

[0115] Cycles of the present invention can vary in duration. Theduration of a cycle can vary among cycles in a step. A cycle durationis, for example, about 2 minutes to about 90 minutes, about 3 minutes toabout 67 minutes, about 5 minutes to about 45 minutes, about 8 minutesto about 30 minutes, about 10 minutes to about 20 minutes, about 14minutes to about 18 minutes, about 7 minutes to about 9 minutes, about13 minutes to about 15 minutes, about 17 minutes to about 19 minutes,about 28 minutes to about 32 minutes, or about 29 minutes to about 31minutes.

[0116] A cycle can be symmetry or asymmetric. In a symmetric cycle, theperiod of increasing the metal or alloy temperature is equal to theperiod of decreasing the metal or alloy temperature. In an asymmetriccycle, the period of increasing the metal or alloy temperature isdifferent than the period of decreasing the metal or alloy temperature.For an asymmetric cycle, the period of increasing the metal or alloytemperature can be longer than or shorter than the period of decreasingthe metal or alloy temperature.

[0117] For example, in a cycle lasting about 7 minutes to about 9minutes, the temperature can be increased for about 3 minutes and thetemperature can be decreased for about 5 minutes. If the cycle lastsabout 13 minutes to about 15 minutes, the temperature can be increasedfor about 7 minutes and the temperature can be decreased for about 7minutes. If the cycle lasts about 17 minutes to about 19 minutes, thetemperature can be increased for about 9 minutes and the temperature canbe decreased for about 9 minutes. If the cycle lasts about 29 minutes toabout 31 minutes, the temperature can be increased for about 15 minutesand the temperature can decreased for about 15 minutes.

[0118] The number of cycles in a step is generally an integer orhalf-integer value. For example, the number of cycles in a step can beone or more, one to forty, or one to twenty. The number of cycles can be1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19, 20,21, 22, 23, 24, 25, 26, 27, 28, 29, 30, 31, 32, 33, 34, 35, 36, 37, 38,39, or 40. Alternatively, the number of cycles in a step can be 0.5,1.5, 2.5, 3.5, 4.5, 5.5, 6.5, 7.5, 8.5, 9.5, 10.5, 11.5, 12.5, 13.5,14.5, 15.5, 16.5, 17.5, 18.5, 19.5, 20.5, 21.5, 22.5, 23.5, 24.5, 25.5,26.5, 27.5, 28.5, 29.5, or 30.5. In a step comprising a half-integer ora non-integer quantity of cycles, either heating or cooling can occurfirst.

[0119] After the initial heating step, the temperature of a metal or analloy is sufficiently high, such that the temperature is equal to orgreater than the solidus temperature. The solidus temperature variesdepending on the metal or the alloy, and the amount of carbon dissolvedtherein. The temperature at the end of Step (F.) of the third paragraphof the summary is typically about 900° F. to about 3000° F., but variesfrom metal to metal. For example, the temperature at the end of Step(F.) can be about 1932° F. to about 2032° F., about 1957° F. to about2007° F., or about 1932° F. to about 2467° F. for copper; about 2368° F.to about 2468° F, about 2393° F. to about 2443° F., or about 2368° F. toabout 2855° F. for nickel; about 2358° F. to about 2458° F. or about2373° F. to about 2423° F., or about 2358OF to about 2805° F. forcobalt; about 1932° F. to about 2032° F., about 1957° F. to about 2007°F., or about 1932° F. to about 2467° F. for a copper/gold/silver alloy;about 399° F. to about 499° F., about 424° F. to about 474° F., or about399° F. to about 932° F. for a tin/lead/zinc alloy; about 399° F. toabout 499° F., about 424° F. to about 474° F., or about 399° F. to 932°F. for a tin/sodium/potassium/magnesium alloy; about 2550° F. to about2650° F., about 2575° F. to about 2625° F., or about 2550° F to about2905° F. for silicon; about 2058° F. to about 2158° F., about 2073° F.to about 2123° F., or about 2058° F. to about 2855° F. for iron; about2058° F. to about 2158° F., about 2073° F. to about 2123° F., or about2058° F. to about 2855° F. for an iron/vanadium/chromium/manganesealloy; or 2368° F. to about 2468° F., about 2393° F. to about 2443° F.,or about 2368° F. to about 2855° F. for anickel/tantalum/hafnium/tungsten alloy.

[0120] Inert gas or gases can be added during a step. Inert gases arechosen, independently, from the group consisting of argon, nitrogen,helium, neon, xenon, krypton, hydrogen, and mixtures thereof. When aninert gas is added during a step, the inert gas (or mixture thereof) canchange from cycle-to-cycle or within a cycle

[0121] For purposes of the present invention, inert gases used forpurging, particularly in the backspace of a reactor are generallyconsidered separately from the other inert gases. Nitrogen is typicallyadded continuously through a method of the present invention,irrespective of whether “inert gas” flow into the metal is started orstopped. In one example, a nitrogen flow is maintained throughout anentire method, such that a nitrogen pressure of about 0.4-0.6 psi, orabout 0.5 psi is maintained.

[0122] At the end of the instant methods, the molten metal or alloy iscooled. The metal or alloy is cooled, at minimum, to a temperature belowthe solidus temperature. Preferably, the metal or alloy is cooled toroom or ambient temperature. Such cooling can include gradual and/orrapid cooling steps. Gradual cooling typically includes cooling due toheat exchange with air or an inert gas over 1 to 72 hours, 2 to 50hours, 3 to 30 hours, or 8 to 72 hours. Rapid cooling, also known asquenching, typically includes an initial cooling with air or an inertgas to below the solidus temperature, thereby forming a solid mass, andplacing the solid mass into a bath comprising a suitable fluid such astap water, distilled water, deionized water, other forms of water, inertgases (as defined above), liquid nitrogen or other suitable liquifiedgases, a thermally-stable oil (e.g., silicone oil) or organic coolant,and combinations thereof. The bath should contain a suitable quantity ofliquid at a suitable temperature, such that the desired amount ofcooling occurs.

[0123] Methods of the present invention are carried out in a suitablereactor. Suitable reactors are selected depending on the amount of metalor alloy to be processed, mode of heating, extent of heating(temperature) required, and the like. A preferred reactor in the presentmethod is an induction furnace reactor, which is capable of operating ina frequency range of 0 kHz to about 10,000 kHz, 0 kHz to about 3,000kHz, or 0 kHz to about 1,000 kHz. Reactors operating at lowerfrequencies are desirable for larger metal charges, such that a reactoroperating at 0-3,000 kHz is generally suitable for 20 pound metalcharges and a reactor operating at 0-1,000 kHz is generally suitable for5000 pound metal charges.

[0124] Typically, reactors of the present method are lined with asuitable crucible. Crucibles are selected, in part, based on the amountof metal or alloy to be heated and the temperature of the method.Crucibles selected for the present method typically have a capacity fromabout five pounds to about five tons. One preferred crucible iscomprised of 89.07% Al₂O₃, 10.37% SiO₂, 0.16% TiO₂, 0.15% Fe₂O₃0.03%CaO, 0.01% MgO, 0.02% Na₂O₃, and 0.02% K20, and has a 9″ outsidediameter, a 7.75″ inside diameter, and a 14″ depth. A second preferredcrucible is comprised of 99.68% Al₂O₃, 0.07% SiO₂, 0.08% Fe₂O₃, 0.04%CaO, and 0.12% Na₂O₃, and has a 4.5″ outside diameter, a 3.75″ insidediameter and a 10″ depth.

[0125] After being subjected to a process of the present invention,metals and alloys can be analyzed by a variety of techniques, includingchemical and physical methods. A preferred analytical method is x-rayfluorescence spectrometry. X-ray fluorescence spectrometry is describedin “X-Ray Fluorescence Spectrometry”, by George J. Havrilla in “Handbookof Instrumental Techniques for Analytical Chemistry,” Frank A. Settle,Ed., Prentice-Hall, Inc: 1997, which is incorporated herein byreference.

[0126] XRF spectrometry is a well-known and long-practiced method, whichhas been used to detect and quantify or semi-quantify the elementalcomposition (for elements with Z≧11) of solid and liquid samples. Thistechnique benefits from minimal sample preparation, wide dynamic range,and being nondestructive. Typically, XRF data are not dependent on whichdimension (e.g., axial or radial) of a sample was analyzed. Accuracy ofless than 1% error can generally be achieved with XRF spectrometry, andthe technique can have detection limits of parts per million.

[0127] XRF spectrometry first involves exciting an atom, such that aninner shell electron is ejected (e.g., the photoelectric effect). Uponejection of an electron, an outer shell electron will “drop” down intothe lower-energy position of the ejected inner shell electron. When theouter shell electron “drops” into the lower-energy inner shell, x-rayenergy is released. Typically, an electron is ejected from the K, L, orM shell and is replaced by an electron from the L, M, or N shell.Because there are numerous combinations of ejections and replacementspossible for any given element, x-rays of several energies are emittedduring a typical XRF experiment. Therefore, each element in the PeriodicTable has a standard pattern of x-ray emissions after being excited by asufficiently energetic source, since each such element has its owncharacteristic electronic state. By matching a pattern of emitted x-rayenergies to values found in tables, such as those on pages 10-233 to10-271 of “Handbook of Chemistry and Physics, 73 ^(rd) Edition,” editedby D. R. Lide, CRC Press, 1992, which is incorporated herein byreference, one can identify which elements are present in a sample. Inaddition, the intensity of the emitted x-rays allows one to quantify theamount of an element in a sample.

[0128] There are two standard variations of the XRF technique. First, asan energy-dispersive method (EDXRF), the XRF technique uses a detectorsuch as a Si(Li) detector, which is capable of simultaneously measuringthe energy and intensity of x-ray photons from an array of elements.EDXRF is well-suited for rapid acquisition of data to determine grosselemental composition. Typically, the detection limits for EDXRF are inthe range of tens to hundreds of parts-per-million. Awavelength-dispersive technique (WDXRF) is generally better-suited foranalyses requiring high accuracy and precision. WDXRF uses a crystal todisperse emitted x-rays, based on Bragg's Law. Natural crystals, such aslithium fluoride and germanium, are commonly used for high-energy (shortwavelength) x-rays, while synthetic crystals are commonly used forlow-energy (longer wavelength) x-rays. Crystals are chosen, in part, toachieve desired resolution, so that x-rays of different energies aredisperse to distinguishable 2 θ angles. WDXRF can either measure x-rayssequentially, such that a WDXRF instrument will step through a range of2 θangles in recording a spectrum, or there will be detectors positionedat multiple 2 θangles, allowing for more rapid analysis of a sample.Detectors for WDXRF commonly include gas ionization and scintillationdetectors. A further description of the use WDXRF technique in thepresent invention can be found in Example 1. Results from EDXRF andresults from WDXRF can be compared by determining the relationshipbetween a 2 θ angle and the wavelength of the corresponding x-ray (e.g.,using Bragg's Law) and converting the wavelength into an energy (e.g.,energy equals wavelength multiplied by Planck's constant).

[0129] Analysis of emitted x-rays can be carried out automatically orsemi-automatically, such as by using a software package (e.g., UniQuant,which is sold by Omega Data Systems BV, Veldhoven, The Netherlands) foreither EDXRF or WDXRF. UniQuant is used for standardlesssemi-quantitative to quantitative XRF analysis using the intensitiesmeasured by a sequential x-ray spectrometer. The software packageunifies all types of samples into one analytical program. The UniQuantsoftware program is highly effective for analyzing samples for which nostandards are available. Sample preparation is usually minimal or notrequired at all. Samples can be of very different natures, sizes andshapes. Elements from fluorine or sodium up to uranium, or their oxidecompounds, can be analyzed in samples such as a piece of glass, a screw,metal drillings, lubricating oil, loose fly ash powder, polymers,phosphoric acid, thin layers on a substrate, soil, paint, the year ringsof trees, and, in general, those samples for which no standards areavailable. The reporting is in weight % along with an estimated errorfor each element.

[0130] In software packages such as UniQuant, an XRF spectrum iscomposed of data channels. Each data channel corresponds to an energyrange and contains information about the number of x-rays emitted atthat energy. The data channels can be combined into one coherent plot toshow the number or intensity of emitted x-rays versus energy or 2 θangle (the 2 θ angle is related to the wavelength of an x-ray), suchthat the plot will show a series of peaks. An analysis of the peaks byone skilled in the art or the software package can identify thecorrespondence between the experimentally-determined peaks and thepreviously-determined peaks of individual elements. For an element, peaklocation (i.e., the centroid of the peak with respect to energy or 2 θangle), peak profile/shape, peak creation, and peak fluidity would beexpected to be essentially the same, within experimental error, for anysample containing the element. If the same quantity of an element ispresent in two samples, intensity will also be essentially the same,excepting experimental error and matrix effects.

[0131] A typical software package is programmed to correlate certaindata channels with the emitted x-rays of elements. Quantification of theintensity of emitted x-rays is accomplished by integrating the XRFspectrum over a number of data channels. Based on the measuredintensities and the previously-compiled data on elements, the softwarepackage will integrate over all data channels, correlate the emittedx-ray intensities, and will then calculate the relative abundance orquantity of elements which appear to be present in a sample, based uponcomparison to the standards. Ideally, the relative abundances will total100% prior to normalization. However, for a variety of reasons, such asimproper or insufficient calibration, the relative abundances will nottotal 100% prior to normalization. Another reason that the relativeabundances of elements do not total 100% prior to normalization is thata portion of the XRF spectrum falls outside of the data channels thatthe software package correlates with an element (i.e., a portion of theXRF spectrum is not recognized as belonging to an element and is notincluded in the relative abundance calculation). In this case, therelative abundances will likely total less than 100% prior tonormalization. Representative examples of relative abundance data arepresented in Table 4, which includes the results of XRF analyses of theproducts of Examples 1-10, as processed by a Uniquant software package.

[0132] X-ray emission spectrometry (XES), a technique analogous to XRF.,also provides electronic information about elements. In XES, alower-energy source is used to eject electrons from a sample, such thatonly the surface (to several micrometers) of the sample is analyzed.Similar to XRF., a series of peaks is generated, which corresponds toouter shell electrons replacing ejected inner shell electrons. The peakshape, peak fluidity, peak creation, peak intensity, peak centroid, andpeak profile are expected to be essentially the same, withinexperimental error and matrix effects, for two samples having the samecomposition.

[0133] A new composition of matter of the present invention can manifestitself as a transient, adjustable, or permanent change in energy and/orassociated properties, as broadly defined. Property change can beexhibited as or comprise a change in: (1) structural atomic character(e.g., XES/XRF peak creation, peak fluidity, peak intensity, peakcentroid, peak profile or shape as a function of material/sampleorientation, atomic energy level(s), and TEM, STM, MFM scans); (2)electronic character (e.g., electron electromagnetic interactions,electromagnetic field position/orientation, energy gradients, Halleffect, voltage, capacitance, voltage decay rate, voltage gradient,voltage signature including slope of decay and/or change of slope decay,voltage magnitude, voltage orientation); (3) structural molecular oratomic character (e.g, SEM, TEM, STM, AFM, LFM, and MFM scans, opticalmicroscopy images, and structural orientation, ordering, long rangealignment/ordering, anisotropy); (4) physical constants (e.g., color,crystalline form, specific rotation, emissivity, melting point, boilingpoint, density, refractive index, solubility, hardness, surface tension,dielectric, magnetic susceptibility, coefficient of friction, x-raywavelengths); (5) physical properties (e.g., mechanical, chemical,electrical, thermal, engineering, and the like); and, (6) other changesthat differentiate naturally occurring materials from manufacturedmaterials created by inducing a change in matter.

[0134] 1. Structural Atomic Character

[0135] In the sections below, certain analyses have been conducted wherea block of a manufactured product (e.g., a metal or an alloy) has beencut from a larger piece. In these analyses, the axial direction or anaxial trace refers. to a side of the block that was originally parallelto the side walls of a reactor. The radial direction or a radial tracerefers to a side of the block that was originally parallel with the topor bottom of a reactor. A metal block can also contain micro- ormacro-voids that can be analyzed.

[0136]FIG. 1A shows a non-contact, magnetic force microscopy image ofnatural copper, the control standard, and FIG. 1B shows a newcomposition of matter: manufactured copper, which is identified by analtered and aligned electromagnetic network. FIG. 2A shows anon-contact, magnetic force microscopy (MFM) scan and FIG. 2B shows ascanning tunneling microscopy (STM) scan. Individually, and fromdiffering vantage points, these scans show the outline of the changedelectromagnetic energy network. The MFM scan shows the radial tracewhile the STM scan shows the axial trace.

[0137] XES analysis of the control standard compared to the atomicallyaltered (i.e., manufactured) state are shown in FIGS. 3A, 3B, 4A, and4B. Manufactured copper in the axial direction exhibits similarcomposition to natural copper (i.e., 99.98%_(wt)), but radial scansexhibit new peaks in the region close to naturally occurring S, Cl, andK. The shifting centroid of the observed peaks from the natural species(i.e., S, Cl, K) confirm electronic change in the atomic state of thebase element; as does the non-contact MFM void scan (compare FIG. 1Bwith FIG. 5A). Conventional chemical analysis performed using a LECO(IR) analyzer confirmed the absence of sulfur at XES lower detectionlimits. LECO analysis confirmed sulfur concentration at 7.8 ppm; thisanalysis was consistent with the manufacture's batch product analysis of7.0 ppm S.

[0138]FIG. 5B compares the XES radial scan of manufactured copper tothat of a void space within the same material. An underlying change inatomic character can be inferred from a dramatic change in signalcount/intensity and a non-contact MFM of the void space (FIG. 5A). MFMevidence highlights the structure and its changed orientation andalignment compared to the control MFM (FIG. 1A).

[0139] High precision XRF imaging shows that manufactured copper has aK_(α) line in the vicinity of 110.7 degrees (the 2 θ angle). Since 110.7degrees is the location of natural sulfur's K_(α) line, this K_(α) lineis referred to herein as a “sulfur-like” K_(α) line. This is the K_(α)line that would be expected if detectable quantities of sulfur werepresent; however, an IR LECO analysis of this sample showed that therewas no sulfur was present (<10 ppm) in the sample. The presence of thisline indicates an electronic structure change, which has shifted the twotheta degree position of the K_(α) line compared to natural copper(FIGS. 6A and 6B). Several other figures indicate the presence ofunexpected K_(α) lines for elements not present in the sample (e.g.,FIG. 27 shows the presence of a significant aluminum-like K_(α) line fora sample containing 99.98% copper). FIG. 7 shows an increase in signalintensity dependent upon which side of a homogeneous block of sample wasanalyzed, as well as a shifting K_(α) centroid. These data demonstratemicroscopically the bulk anisotropy later identified in the manufacturedsample as does the MFM scans (FIGS. 1B and 5A).

[0140] 2. Electronic Character

[0141] Manipulation of the electrodynamic components affecting theorientation of a manufactured metal's or alloy's electromagnetic fieldcan enable the observance of a Hall voltage (V_(H)). Manipulation of theelectrodynamic components enables intensification of electromagneticfield affording charge concentration on the surface of the atoms withinthe bulk as opposed to the bulk surface of the bath. Properties thatreflect field repositioning can include changing capacitance and voltagedecay rate (FIG. 8) and voltage gradients (FIG. 9) within a conductingbulk media.

[0142]FIG. 10 shows the V_(H) observed in a copper-nickel alloy. Voltagedecay exhibited two distinct decay rates, indicative of two controllingmechanisms. A positive voltage signature with a positive capacitancedecay (i.e., capacitance accumulation) is shown in FIG. 11.

[0143] Control and manipulation of the charge signature (e.g., V_(H)Profile, capacitance slope, voltage slope) provides evidence of thealteration, and manipulation of the underlying electronic state. FIG. 12shows a positive voltage signature and a positive capacitance decay.Additionally, the voltage decay profile has changed: one profile has anegative slope while the other has a neutral slope. Further change inthe electronic structure enables the slope of the second voltage decayprofile to become positive (FIG. 13); note also the change in slope ofcapacitance decay. The metal system shown in FIG. 14 has an electronicstructure change that result in a nearly neutral decay in voltage andcapacitance. Measurements were repeated four times. FIG. 15 shows thatthe voltage can actually become negative, indicating that theorientation can also be manipulated. FIG. 16 shows the phenomena can beobserved under pressure. Table 1 is an XRF analysis using a Uniquantsoftware package that shows a multiplicity of energetically contiguousX-ray atomic energy levels. One energetically contiguous series isrepresented by Sm, Eu, Gd, Th; the other is represented by P, S, So(i.e., sulfur as an oxide), Cl, and Ar. Table 2 is an XRF analysis usinga Uniquant software package that shows an energetically contiguousseries as Al, Si, P, S, So (i.e., sulfur as an oxide), Cl, Ar, K, andCa. Table 3 represents an experiment that utilized the same startingmaterial as Tables 1 and 2, however, the reported amount or abundance ofcopper after processing differs from the other tables. The differingrelative abundances of elements observed in Tables 1-3 are believed tocorrespond to the unexpected peaks seen in many of the XRF plots.

[0144] 3. Structural Molecular/Atomic Character

[0145] New compositions of matter can be electronically modified toinduce long range ordering/alignment. In one new composition of matter,long range ordering was induced in oxygen-free high conductivity (OFHC)copper. Optical microscopy and SEM imaging of the material verifies thedegree and extent of long range ordering achieved (FIGS. 17A, 17B, 17C,18A, 18B, and 18C). Under similar electronic conditions, long rangeordering was induced in high purity (99.99 %_(wt)) nickel. FIGS. 19A,19B, 20A, and 20B show the optical microscopy imaging of themanufactured nickel material. A comparison of alignment is shown in-run,at two different points during processing, which highlights theadjustability of the altered electronic state of the manufacturednickel.

[0146] Extensive atomic force microscopy and non-contact MFM imaging ofelectronically altered OFHC copper shows views of structuralconfigurations from a different perspective (FIG. 21A, 21B, 21C, 22A,22B, and 22C). Non-contact MFM imaging shows clear pattern repetitionand intensity of the manufactured copper when compared to the naturalcopper. The manufactured copper represents a new composition of matterderived from natural copper, and the manufactured copper exhibitsanisotropic behavior.

[0147] 4. Physical Constants

[0148] In one sequence of new compositions of matter, color changes inOFHC copper were induced. The variation in color over four (4) newmatter compositions ranged from black (two intensities) to copper (2intensities) to gold (one intensity) to silver (one intensity). Whilenot being bound by theory, the alteration of copper's electronic statealong the continuum enables the new composition of matter's color to beadjusted along the continuum.

[0149] In another sequence of new compositions of matter, changes in thehardness of OFHC copper were induced. The variation in diamond pyramidhardness between different manufactured copper samples ranged from about25 to 90 (or 3 to 9 times higher than natural copper). Hardness changewas anisotropic.

[0150] In another new composition of matter, magnetism was induced in ahigh purity, non-magnetic metal copper (e.g., 99.98 %_(wt)) in itselemental form (FIGS. 23A and 23B).

[0151] 5. Physical Properties

[0152] In one sequence of new compositions of matter, ductility changeswere induced in a high purity, ductile copper (99.98%_(wt)) in itselemental form. The variation in the engineering physical property ofductility ranged from brittle to semi-ductile to ductile to extremelyductile over four (4) new matter compositions.

[0153] In one new composition of matter, the electrical reactance wasincreased approximately 3% above that of natural copper over thefrequency range of 0 Hz to 100 kHz. In another new composition ofmatter, electrical susceptance was increased approximately 20% above99.98%_(wt) copper of the same chemical composition (i.e., the copper inits natural state). In another new composition of matter, electricalsusceptance was decreased approximately 25% below 99.98%_(wt) copper ofthe same chemical composition (i.e., the copper in its natural state).Electrical susceptance for these new matter compositions compared to thecontrol standard (the material in its natural state) is shown in FIG.24.

[0154] 6. Additional Differentiations

[0155] In one sequence of new compositions of matter, which all used thesame raw materials, consumables, utilities, and materials ofconstruction, the sum of element concentrations identified by XRFanalysis varied considerably. Variations in elemental abundancedetermined by XRF Uniquant prior to normalization over three (3) newmatter compositions were 99.5 %_(wt) (Table 3), 96.0 %wt (Table 2), and90.6%_(wt) (Table 1). The apparent loss of matter between the recognizedelemental structures and the manufactured elemental structuresdifferentiates naturally occurring materials from materials withmodified electronic structures (i.e., a new composition of matter).

[0156] While not being bound by theory, Applicant believes theconservation of energy requires that all mass, independent of magnitudeand/or configuration, character, and/or dimension can be characterizedby the allowed set of mathematical poles (defined as the operation zurn)and further characterized by the set of mathematical poles coalesced(defined as the isozum value). An adjustment or manipulation of the zuminvokes a change in the isozurn value to a value different than itsnaturally occurring value, and accounts for the contribution of its reststate value, thereby modifying the electronic structure that defines thenatural state. A change in the isozurn value to a value different thanthat which specifies the natural state denotes a change in theunderlying electronic state of the specified species.

[0157] A change in the isozurn value is typically noted at thesubatomic, atomic, or molecular level. While not being bound by theory,the complexity of energy interactions is believed to often impede singlevariable isolation. In these cases, a change in the electronic state ofthe specified species typically manifests itself as a change in aproperty value(s) from the naturally occurring state (e.g., theunaltered entropic driven ground state). Typical changes denoting achange in property value, which depart from the property valuespecifying its naturally occurring state, dictate a change in theisozurn value of that state.

[0158] Definitions of Acronyms

[0159] AO—Atomic Orbital

[0160] SEM—Scanning electron microscopy

[0161] TEM—Tunneling Electron Microscopy

[0162] STM—Scanning Tunneling Microscopy

[0163] AFM—Atomic Force Microscopy

[0164] LFM—Lateral Force Microscopy

[0165] MFM—Magnetic Force Microscopy

[0166] XES—X-ray Emission Spectrometry

[0167] XRF—X-ray Fluorescence Spectrometry

EXEMPLIFICATION EXAMPLE 1 Experimental Procedure for Copper Run 14-01-01

[0168] A cylindrical alumina-based crucible (99.68% Al₂O₃, 0.07% SiO₂,0.08% Fe₂O₃, 0.04% CaO, 0.12% Na₂O₃; 4.5″ O.D.×3.75″ I.D.×10″ depth) ofa 100 pound induction furnace reactor (Inductotherm) fitted with a 75-30R Powertrak power supply was charged with 2500 g copper (99.98% purity)through its charging port. The reactor was fitted with a graphite capand a ceramic liner (i.e., the crucible, from Engineering Ceramics).During the entire procedure, a slight positive pressure of nitrogen(˜0.5 psi) was maintained in the reactor using a continuous backspacepurge. The reactor was heated to the metal charge liquidus point plus300° F., at a rate no greater than 300° F./hour, as limited by theintegrity of the crucible. The induction furnace operated in thefrequency range of 0 kHz to 3000 kHz, with frequency determined by atemperature-controlled feedback loop implementing an Omega Model CN300temperature controller. Upon reaching 2300° F., the reactor was chargedwith an additional 2143 g copper over an hour.

[0169] The temperature was again increased to 2462° F. again using arate no greater than 300° F./hour. When this temperature was reached,graphite saturation assemblies (⅜″ OD, 36″ long high purity (<5 ppmimpurities) graphite rods) were inserted to the bottom of the coppercharge through ports located in the top plate. The copper was held at2462° F. for 4 hours. Every 30 minutes during the hold period, anattempt was made to lower the graphite saturation assemblies asdissolution occurred. As the copper became saturated with carbon, thegraphite saturation assemblies were consumed. After the 4 hour holdperiod was complete, the graphite saturation assemblies were removed.

[0170] The reactor temperature was increased to 2480° F. over 7 minutes.The temperature was then varied between 2480° F. and 2530° F. for 15cycles. Each cycle consisted of raising the temperature continuouslyover 7 minutes and lowering the temperature continuously over 7 minutes.After the 15 cycles were completed, a gas addition lance was loweredinto the molten metal to a position approximately 2″ from the bottom ofthe reactor and a 0.15 L/min flow of argon was begun. The temperature ofthe copper was varied over another 5 cycles between 2480° F. and 2530°F.

[0171] After the fifth cycle, the reactor temperature was lowered to2462° F. over a 10 minute period with continued argon addition. Thegraphite saturation assemblies were reinstalled in the copper andremained there for 1 hour. The graphite saturation assemblies wereremoved.

[0172] The reactor temperature was lowered to 2459° F. over 5 minutes.The reactor was held at this temperature for 5 minutes with continuedargon addition. The temperature was then varied between 2459° F. and2453° F. over 20 cycles. Each cycle consisted of lowering thetemperature continuously over 9 minutes and raising the temperaturecontinuously over 9 minutes. The argon addition ceased after completionof the 20 cycles.

[0173] The reactor temperature was lowered to 2450° F. over 5 minutes.The temperature was varied between 2450° F. and 2441° F. over 4½ cycles.Each cycle consisted of lowering the temperature continuously over 5minutes and raising the temperature continuously over 3 minutes. Inaddition, while raising the temperature, a 0.15 L/min flow of argon wasadded, and while lowering the temperature, a 0.15 L/min flow of nitrogenwas added.

[0174] The reactor temperature was lowered to 2438° F. over 5 minutes.The temperature was varied between 2438° F. and 2406° F. for 15.5cycles. Each cycle consisted of lowering the temperature continuouslyover 15 minutes and raising the temperature continuously over 15minutes. In addition, while raising the temperature, a 0.15 L/min flowof argon was added, and while lowering the temperature, a 0.15 L/minflow of nitrogen was added. All gas addition, except for the purge ofnitrogen ceased after the 15.5 cycles were completed.

[0175] The temperature was varied between 2406° F. and 2419° F. for onecycle. The cycle consisted of raising the temperature continuously over15 minutes and lowering the temperature continuously over 15 minutes.The gas addition lance was removed.

[0176] The reactor temperature was cooled by lowering the inductionfurnace power to 1 kW or less as the ingot cooled. The copper was thencooled to approximately ambient temperature in water.

ANALYTICAL PROTOCOLS

[0177] X-ray Fluorescence

[0178] An ARL 8410 XRF was used to analyze each of the sample ingots. AnARL 8410 is a sequential wavelength dispersive spectrometer (WDS).Specific emission lines are used to determine the presence or absence,and the concentrations of various elements. Each characteristic x-rayline is measured in sequence by the instrument by controlling theinstrument geometry.

[0179]FIG. 62 shows the general configuration of the ARL 8410spectrometer. The WDS spectrometer relies on the fundamentals of x-raydiffraction, when x-ray fluorescence occurs when matter is bombarded bya stream of high-energy incident x-ray photons. When the incidentX-radiation strikes the sample, the incident x-rays may be absorbed,scattered, or transmitted for the measurement of the fluorescent yield.

[0180] The ARL 8410 utilizes an end-window rhodium (Rh) x-ray tube. Theend-window is composed of Be, and holds the tube at high vacuum. Thefilaments are heated giving off electrons by thermoionic emission. Thisbeam of electrons then bombards the target Rh anode across a 10-70 keVvoltage potential. Thus, primary x-rays are produced during thecollision. The emitted x-ray spectrum consists of (1) “Continuum” or“Bremstrahlung” radiation, (2) Characteristic x-ray lines of the targetmaterial (e.g., K and L series), and (3) Characteristic lines from anycontaminants. Thus, the primary spectrum appears as a series of sharpintense peaks arrayed over a broad hump of continuum radiation. The ARLis equipped with and uses two types of photon detectors, the FlowProportional Counter (FPC) and the Scintillation Counter (SC).

[0181] The manufactured metal samples are prepared by cutting a cubeshape (approximately 1.1875 ″) from the center of the cooled ingot. Anaxial edge and a radial edge are then denoted. To provide a smoothsurface for analysis, the axial and radial faces are sequentiallypolished. The sample faces are sanded to 400 grit, then a polishingwheel is employed with 600 grit paper. Finally, a ≦1 μm polishingcompound completes the smoothing process. The sample is then cleanedwith iso-propyl alcohol and placed in a sample cassette/holder. Thesample holder is then loaded into the XRF.

[0182] The orientation of the detector crystal with respect to thesample and the photon detector is controlled synchronously such thatcharacteristic x-ray lines can be accurately measured. A sequentialmeasurement consists of positioning the diffraction crystal at a giventheta (diffraction angle) and the detector at two-theta and counting fora given period of time. The crystal and detector are then rotated to adifferent angle for the next characteristic x-ray line.

[0183] Uniquant Version 2 software, developed by Omega Data Systems isused to control the crystal and detector placement and provides the datareduction algorithms for each analytical protocol. The sample resultsinclude an elemental i composition list along with the associatedconcentrations for each sample.

[0184] Measurement of Grain Sizes

[0185] When the grain sizes exceeded the size discernible with the humaneye, the grain size (average span distance) was measured using amicrometer. When the grain sizes were not discernible via the naked eye,standard acid etching was performed and then optical microscopy wasutilized to measure and characterize the grain.

[0186] Measurement of Magnetism

[0187] The magnetic properties of the manufactured ingots were testedvia three methods.

[0188] Magnetic Attraction: An ⅛″ diameter neodymium iron boron magnetwas scanned consistently and uniformly across the surface of the ingotto detect areas of attraction. Areas of attraction were then noted atspecific sites on the surface.

[0189] Attraction to Iron: The attraction of iron filings to specificpoints on the ingot were quantified by enumerating the number of filingsretained on the ingot surface in a vertical or upside-down orientation.

[0190] Gauss Measurement: The magnetic behavior of various points on theingot were quantified via the use of a F.W. Bell 4048 Gauss meter.

[0191] Measurement of Chemical Reactivity

[0192] The manufactured ingots were subjected to various chlorineligands, including NaCl, NaOCl, HCl, and chlorinated organics tosemi-quantitatively access their reactivity to ligated chlorine. Theformation of reaction products was recorded, then reaction products wereremoved from the reaction site, weighed and elemental compositionverified via XRF.

ANALYTICAL RESULTS

[0193] An x-ray fluorescence analysis of the copper sample is providedin FIG. 26, with the K_(α) peak of a copper control standard shown forreference.

[0194] An x-ray fluorescence analysis of the copper sample is providedin FIG. 27, with the K_(α) peak of an aluminum control standard shownfor reference.

[0195] Summary data showing the apparent elemental composition of theproduct of Example 1 is shown in Tables 5-13, as was measured by an XRFanalysis using a Uniquant software package. The apparent elementalcomposition of the product varies by position, which is indicated ineach table.

[0196] The manufactured copper exhibited large grain sizes and differentcoloration on each grain, which caused the surface to appear iridescent.The axial (top) face of the ingot appeared glassy, while the sides weremetallic in appearance (due to anisotropic behavior). The color on boththe axial and radial surfaces mimicked that of natural copper (i.e., notthe intense reds or dark browns observed in other manufactured coppers,for example, Examples 11-14). On the axial surface, unique demarcationswere observed. The ingot had some internal void areas, which were opento the top surface. No unexpected magnetic activity or chemicalreactivity were recorded.

EXAMPLE 2 Experimental Procedure for Nickel Run 14-01-04

[0197] A cylindrical alumina-based crucible (99.68% Al₂O₃, 0.07% SiO₂,0.08% Fe₂O₃, 0.04% CaO, 0.12% Na₂O₃; 4.5″ O.D.×3.75″ I.D.×10″ depth) ofa 100 pound induction furnace reactor supplied by Inductotherm, wasfitted with a 75-30 R Powertrak power supply and charged with 2500 gnickel (99.97% purity) and 100 g of graphite carbon through its chargingport. The reactor was fitted with a graphite cap with a ceramic liner(i.e. the crucible, from Engineering Ceramics). During the entireprocedure, a slight positive pressure of nitrogen (˜0.5 psi) wasmaintained in the reactor using a continuous backspace purge. Thereactor was heated to the metal charge liquidus point, over a rate nogreater than 300° F./hour, as limited by the integrity of the crucible.The induction furnace operated in a frequency range of 0 kHz to 3000kHz, with frequency determined by a temperature-controlled feedback loopimplementing an Omega Model CA 300 temperature controller. Upon reaching2800° F., the reactor was charged with an additional 2700 g nickel overan hour.

[0198] The temperature was again increased to 2850° F. again using arate no greater than 300° F./hour. When this temperature was reached,graphite saturation assemblies (⅜″ OD, 36″ long high purity [<5 ppmimpurities] graphite rods) were inserted to the bottom of the nickelcharge through ports located in the top plate. The nickel was held at2850° F. for 4 hours. Every 30 minutes during the hold period, anattempt was made to lower the graphite saturation assemblies asdissolution occurred. As the nickel became saturated with carbon, thegraphite saturation assemblies were consumed. After the 4 hour holdperiod was complete, the graphite saturation assemblies were removed.

[0199] The reactor temperature was increased to 3256° F. over 7 minutes.The temperature was then varied between 2950° F. and 3256° F. for 15cycles. Each cycle consisted of lowering the temperature continuouslyover 7 minutes and raising the temperature continuously over 7 minutes.After the 15 cycles were completed, a gas addition lance was lowered anda 0.15 L/min flow of argon was begun. The temperature of the nickel wasvaried over another 5 cycles between 2950° F. and 3256° F.

[0200] After the fifth cycle, the reactor temperature was lowered to2850° F. over a 10 minute period with continued argon addition. Thegraphite saturation assemblies were reinstalled in the nickel andremained there for 1 hour. The graphite saturation assemblies wereremoved.

[0201] The reactor temperature was lowered to 2829° F. over 5 minutes.The reactor was held at this temperature for 5 minutes with continuedargon addition. The temperature was then varied between 2790° F. and2829° F. over 20 cycles. Each cycle consisted of lowering thetemperature continuously over 9 minutes and raising the temperaturecontinuously over 9 minutes. The argon addition ceased after completionof the 20 cycles.

[0202] The reactor temperature was lowered to 2770° F. over 5 minutes.The temperature was varied between 2710° F. and 2770° F. over 4½ cycles.Each cycle consisted of lowering the temperature continuously over 5minutes and raising the temperature continuously over 3 minutes. Inaddition, while raising the temperature, a 0.15 L/min flow of argon wasadded, and while lowering the temperature, a 0.15 L/min flow of nitrogenwas added.

[0203] The reactor temperature was lowered to 2691° F. over 5 minutes.The temperature was varied between 2492° F. and 2691° F. for 15.5cycles. Each cycle consisted of lowering the temperature continuouslyover 15 minutes and raising the temperature continuously over 15minutes. In addition, while raising the temperature, a 0.15 L/min flowof argon was added, and while lowering the temperature, a 0.15 L/minflow of nitrogen was added. All gas addition, except for the purge ofnitrogen ceased after the 15.5 cycles were completed.

[0204] The temperature was varied between 2571° F. and 2492° F. for onecycle. The cycle consisted of raising the temperature continuously over15 minutes and lowering the temperature over 15 minutes. The gasaddition lance was removed.

[0205] The reactor temperature was slowly cooled by lowering theinduction furnace power to 1 KW or less as the ingot cooled. The nickelwas then cooled to approximately ambient temperature in water.

ANALYTICAL PROTOCOLS

[0206] XRF, grain size, magnetism, and chemical reactivity measurementswere carried out by the procedures described in Example 1.

ANALYTICAL RESULTS

[0207] An x-ray fluorescence analysis of the nickel sample is providedin FIGS. 28A and 28B, with the K_(α) and L_(α) peaks of a nickel controlstandard shown for reference.

[0208] An x-ray fluorescence analysis of the nickel sample is providedin FIG. 29A, with the K_(α) peak of an aluminum control standard shownfor reference.

[0209] An x-ray fluorescence analysis of the nickel sample is providedin FIG. 29B, with the K_(α) peak of a zirconium control standard shownfor reference.

[0210] An x-ray fluorescence analysis of the nickel sample is providedin FIG. 30A, with the K_(α) peak of a sulfur control standard shown forreference.

[0211] An x-ray fluorescence analysis of the copper sample is providedin FIG. 30B, with the K_(α) peak of an chlorine (from potassiumchloride) shown for reference.

[0212] Summary data showing the apparent elemental composition of theproduct of Example 2 is shown in Tables 14-16, as was measured by an XRFanalysis using a Uniquant software package. The apparent elementalcomposition of the product varies by position, which is indicated ineach table.

[0213] The manufactured nickel retained a large amount of refractory onits exterior surface after retrieval from the reactor. The retainedrefractory was attributed to either surface attraction or reaction withthe high content of Al₂O₃ in the refractory. The ingot did not crackwith handling, but did have an internal void. The visible radial surfaceappeared duller in than the axial (top) face, again demonstratinganisotropic physical properties. The ingot demonstrated no unexpectedchemical reactivity after removal from the reaction system.

EXAMPLE 3 Experimental Procedure for Cobalt Rrun 14-01-05

[0214] A cylindrical alumina-based crucible (99.68% Al₂O₃, 0.07% SiO₂,0.08% Fe₂O₃, 0.04% CaO, 0.12% Na₂O₃; 4.5″ O.D.×3.75″ I.D. x 10″ depth)of a 100 pound induction furnace reactor supplied by Inductotherm andfitted with a 75-30 R Powertrak power supply, was charged with 2176 gcobalt (99.8% purity) through its charging port. The reactor was fittedwith a graphite cap with a ceramic liner from Engineering Ceramics.During the entire procedure, a slight positive pressure of nitrogen(˜0.5 psi) was maintained in the reactor using a continuous backspacepurge. The reactor was heated to 2800° F. over a minimum of 14 hourswhile the induction furnace operated in a frequency range of 0 kHz to3000 kHz. Upon reaching 2700° F., the reactor was charged with anadditional 3000 g cobalt over an hour.

[0215] When 2800° F. was reached, graphite saturation assemblies wereinserted to the bottom of the cobalt charge through ports located in thetop plate. The cobalt was held at 2800° F. for 4 hours. Every 30 minutesduring the hold period, an attempt was made to lower the graphitesaturation assemblies as dissolution progressed. As the cobalt becamesaturated with carbon, the graphite saturation assemblies were consumed.After the 4 hour hold period was complete, the graphite saturationassemblies were removed.

[0216] The reactor temperature was increased to 3086° F. over 7 minutes.The temperature was then varied between 2875° F. and 3086° F. for 15cycles. Each cycle consisted of lowering the temperature continuouslyover 7 minutes and raising the temperature continuously over 7 minutes.After the 15 cycles were completed, a gas addition lance was lowered anda 0.15 L/min flow of argon was begun. The temperature of the cobalt wasvaried over another 5 cycles between 2875° F. and 3086° F.

[0217] After the fifth cycle, the reactor temperature was lowered to2800° F. over a 10 minute period with continued argon addition. Thegraphite saturation assemblies were reinstalled in the cobalt andremained there for 1 hour. The graphite saturation assemblies wereremoved.

[0218] The reactor temperature was lowered to 2785° F. over 5 minutes.The reactor was held at this temperature for 5 minutes with continuedargon addition. The temperature was then varied between 2689° F. and2785° F. over 20 cycles. Each cycle consisted of lowering thetemperature continuously over 9 minutes and raising the temperaturecontinuously over 9 minutes. The argon addition ceased after completionof the 20 cycles.

[0219] The reactor temperature was lowered to 2737° F. over 5 minutes.The temperature was varied between 2689° F. and 2737° F. over 4½ cycles.Each cycle consisted of lowering the temperature continuously over 5minutes and raising the temperature continuously over 3 minutes. Inaddition, while raising the temperature, a 0.15 L/min flow of argon wasadded, and while lowering the temperature, a 0.15 L/min flow of nitrogenwas added.

[0220] The reactor temperature was lowered to 2672° F. over 5 minutes.The temperature was varied between 2498° F. and 2672° F. for 15.5cycles. Each cycle consisted of lowering the temperature continuouslyover 15 minutes and raising the temperature continuously over 15minutes. In addition, while raising the temperature, a 0.15 L/min flowof argon was added, and while lowering the temperature, a 0.15 L/minflow of nitrogen was added. All gas addition, except for the purge ofnitrogen ceased after the 15.5 cycles were completed.

[0221] The temperature was varied between 2570° F. and 2498° F. for onecycle. The cycle consisted of raising the temperature continuously over15 minutes and lowering the temperature continuously over 15 minutes.The gas addition lance was removed.

[0222] The reactor temperature was cooled by. lowering the inductionfurnace power to 1 kW or less as the ingot cooled. The cobalt was thencooled to approximately ambient temperature in water.

ANALYTICAL PROTOCOLS

[0223] XRF, grain size, magnetism, and chemical reactivity measurementswere carried out by the procedures described in Example 1.

ANALYTICAL RESULTS

[0224] An x-ray fluorescence analysis of the cobalt sample is providedin FIGS. 31A and 31B, with the K_(α) and L_(α) peaks of a cobalt controlstandard shown for reference.

[0225] An x-ray fluorescence analysis of the cobalt sample is providedin FIG. 32A, with the K_(α) peak of an aluminum control standard shownfor reference.

[0226] An x-ray fluorescence analysis of the cobalt sample is providedin FIG. 32B, with the K_(α) peak of an iron control standard shown forreference.

[0227] An x-ray fluorescence analysis of the cobalt sample is providedin FIG. 33A, with the K_(α) peak of a chlorine (from potassium chloride)control standard shown for reference.

[0228] An x-ray fluorescence analysis of the cobalt sample is providedin FIG. 33B, with the K_(α) peak of a zirconium control standard shownfor reference.

[0229] An x-ray fluorescence analysis of the cobalt sample is providedin FIG. 34, with the K_(α) peak of a manganese control standard shownfor reference.

[0230] Summary data showing the apparent elemental composition of theproduct of Example 3 is shown in Table 17, as was measured by an XRFanalysis using a Uniquant software package.

[0231] The top (axial) face of the manufactured cobalt ingot exhibitedmany of the recursive patterns observed in other manufactured ingots.The surface peaks are inconsistent with what would be expected given theforces of gravity during cooling. In addition, the shiny top face of theingot exhibited an unexpected coloration, such that some of the faceshad a distinct pink tint. While the top of the ingot was shiny, silvermetallic, the sides of the ingot were matte silver in appearance.

[0232] The manufactured cobalt ingot retained a small amount ofrefractory around its base. The ingot did not crack upon retrieval fromthe reaction system. No unexpected magnetic behavior or chemicalreactivity were observed.

EXAMPLE 4 Experimental Procedure for Copper Run 14-01-06

[0233] A cylindrical alumina-based crucible (99.68% Al₂O₃, 0.07% SiO₂,0.08% Fe₂O₃, 0.04% CaO, 0.12% Na₂O₃; 4.5″ O.D.×3.75″ I.D.×10″ depth) ofa 100 pound induction furnace reactor supplied by Inductotherm andfitted with a 75-30 R Powertrak power supply was charged with 2518 gcopper (99.98% purity), plus 62.28 g each of gold (99.9999% pure) andsilver (99.9999% pure) through its charging port. The reactor was fittedwith a graphite cap with a ceramic liner by Engineering Ceramics. Duringthe entire procedure, a slight positive pressure of nitrogen (˜0.5 psi)was maintained in the reactor using a continuous backspace purge. Thereactor was heated to 2300° F. over a minimum of 12 hours while theinduction furnace operated in a frequency range of 0 kHz to 3000 kHz.Upon reaching 2300° F., the reactor was charged with an additional 2000g copper over an hour.

[0234] The temperature was again increased to 2462° F. again using arate no greater than 300° F./hour. When this temperature was reached,graphite saturation assemblies were inserted to the bottom of the metalcharge through ports located in the top plate. The alloy was held at2462° F. for 4 hours. Every 30 minutes during the hold period, anattempt was made to lower the graphite saturation assemblies. As thealloy became saturated with carbon, the graphite saturation assemblieswere consumed. After the 4 hour hold period was complete, the graphitesaturation assemblies were removed.

[0235] The reactor temperature was increased to 2480° F. over 7 minutes.The temperature was then varied between 2480° F. and 2530° F. for 15cycles. Each cycle consisted of raising the temperature continuouslyover 7 minutes and lowering the temperature continuously over 7 minutes.After the 15 cycles were completed, a gas addition lance was lowered anda 0.15 L/min flow of argon was begun. The temperature of the alloy wasvaried over another 5 cycles between 2480° F. and 2530° F.

[0236] After the fifth cycle, the reactor temperature was lowered to2462° F. over a 10 minute period with continued argon addition. Thegraphite saturation assemblies were reinstalled in the alloy andremained there for 1 hour. The graphite saturation assemblies wereremoved.

[0237] The reactor temperature was lowered to 2459° F. over 5 minutes.The reactor was held at this temperature for 5 minutes with continuedargon addition. The temperature was then varied between 2453° F. and2459° F. over 20 cycles. Each cycle consisted of lowering thetemperature continuously over 9 minutes and raising the temperaturecontinuously over 9 minutes. The argon addition ceased after completionof the 20 cycles.

[0238] The reactor temperature was lowered to 2450° F. over 5 minutes.The temperature was varied between 2441° F. and 2450° F. over 4½ cycles.Each cycle consisted of lowering the temperature continuously over 5minutes and raising the temperature continuously over 3 minutes. Inaddition, while raising the temperature, a 0.15 L/min flow of argon wasadded, and while lowering the temperature, a 0.15 L/min flow of nitrogenwas added.

[0239] The reactor temperature was lowered to 2438° F. over 5 minutes.The temperature was varied between 2406° F. and 2438° F. for 15.5cycles. Each cycle consisted of lowering the temperature continuouslyover 15 minutes and raising the temperature continuously over 15minutes. In addition, while raising the temperature, a 0.15 L/min flowof argon was added, and while lowering the temperature, a 0.15 L/minflow of nitrogen was added. All gas addition, except for the purge ofnitrogen ceased after the 15.5 cycles were completed.

[0240] The temperature was varied between 2406° F. and 2419° F. for onecycle. The cycle consisted of raising the temperature continuously over15 minutes and lowering the temperature continuously over 15 minutes.The gas addition lance was removed.

[0241] The reactor temperature was cooled by lowering the inductionfurnace power tol1 kW or less as the ingot cooled. Thecopper/silver/gold was then cooled to approximately ambient temperaturein water.

ANALYTICAL PROTOCOLS

[0242] XRF, grain size, magnetism, and chemical reactivity measurementswere carried out by the procedures described in Example 1.

ANALYTICAL RESULTS

[0243] An x-ray fluorescence analysis of the copper/gold/silver alloysample is provided in FIG. 35, with the K_(α) peak of a copper controlstandard shown for reference.

[0244] An x-ray fluorescence analysis of the copper/gold/silver alloysample is provided in FIG. 36, with the K_(α) peak of a gold controlstandard shown for reference.

[0245] An x-ray fluorescence analysis of the copper/gold/silver alloysample is provided in FIG. 37, with the K_(α) peak of a silver controlstandard shown for reference.

[0246] Summary data showing the apparent elemental composition of theproduct of Example 4 is shown in Tables 18-19, as was measured by an XRFanalysis using a Uniquant software package. The apparent elementalcomposition of the product varies by position, which is indicated ineach table.

[0247] The manufactured copper-based alloy exhibited uniform colorationin both the axial and radial directions. Prior to being quenched inwater, the ingot exhibited significant iridescence on all surfaces.After being quenched, the intensity of iridescence diminished.

[0248] An unexpected feature of the ingot was the axial face crystalorientation. No magnetic behavior was observed. The ingot did not crackor retain any refractory after retrieval from the reactor.

EXAMPLE 5 Eexperimental Procedure for Tin/Lead/Zinc 14-01-07

[0249] A cylindrical alumina-based crucible (99.68% Al₂O₃, 0.07% SiO₂,0.08% Fe₂O₃, 0.64% CaO, 0.12% Na₂O₃; 4.5″ O.D.×3.75× I.D.×10″ depth) ofa 100 pound induction furnace reactor supplied by Inductotherm andfitted with a 75-30 R Powertrak power supply was charged with 2562 gcopper (99.9% purity), plus 854 g each of Lead (99+% pure) and Zinc(99.8% pure) through its charging port. The reactor was fitted with agraphite cap with a ceramic liner by Engineering Ceramics. 30 During theentire procedure, a slight positive pressure of nitrogen (˜0.5 psi) wasmaintained in the reactor using a continuous backspace purge. Thereactor was heated to 932° F. over a minimum of 4 hours at a rate nogreater than 300° F./hour. The induction furnace operated in thefrequency range of 0 kHz to 3000 kHz with frequency determined by atemperature-controlled feedback loop implementing an Omega Model CN300temperature controller.

[0250] When 932° F. was reached, graphite saturation assemblies wereinserted to the bottom of the metal charge through ports located in thetop plate. The tinflead/zinc alloy was held at 932° F. for 4 hours.Every 30 minutes during the hold period, an attempt was made to lowerthe graphite saturation assemblies. As the tin/lead/zinc alloy becamesaturated with carbon, the graphite saturation assemblies were consumed.After the 4 hour hold period was complete, the graphite saturationassemblies were removed.

[0251] The reactor temperature was increased to 968° F. over 7 minutes.The temperature was then varied between 942° F. and 968° F. for 15cycles. Each cycle consisted of lowering the temperature continuouslyover 7 minutes and raising the temperature continuously over 7 minutes.After the 15 cycles were completed, a gas addition lance was loweredinto the molten metal to a position approximately 2″ from the bottom ofthe reactor and a 0.15 L/min flow of argon was begun. The temperature ofthe tin/lead/zinc alloy was varied over another 5 cycles between 942° F.and 968° F.

[0252] After the fifth cycle, the reactor temperature was lowered to932° F. over a 10 minute period with continued argon addition. Thegraphite saturation assemblies were reinstalled in the tin/lead/zincalloy and remained there for 1 hour. The graphite saturation assemblieswere removed.

[0253] The reactor temperature was lowered to 930° F. over 5 minutes.The reactor was held at this temperature for 5 minutes with continuedargon addition. The temperature was then varied between 918° F. and 930°F. over 20 cycles. Each cycle consisted of lowering the temperaturecontinuously over 9 minutes and raising the temperature continuouslyover 9 minutes. The argon addition ceased after completion of the 20cycles.

[0254] The reactor temperature was lowered to 924° F. over 5 minutes.The temperature was varied between 918° F. and 924° F. over 4½ cycles.Each cycle consisted of lowering the temperature continuously over 5minutes and raising the temperature continuously over 3 minutes. Inaddition, while raising the temperature, a 0.15 L/min flow of argon wasadded, and while lowering the temperature, a 0.15 L/min flow of nitrogenwas added.

[0255] The reactor temperature was lowered to 916° F. over 5 minutes.The temperature was varied between 894° F. and 916° F. for 15.5 cycles.Each cycle consisted of lowering the temperature continuously over 15minutes and raising the temperature over 15 minutes. In addition, whileraising the temperature, a 0.15 L/min flow of argon was added, and whilelowering the temperature, a 0.15 LUmin flow of nitrogen was added. Allgas addition, except for the purge of nitrogen ceased after the 15.5cycles were completed.

[0256] The temperature was varied between 894° F. and 903° F. for onecycle. The cycle consisted of raising the temperature continuously over15 minutes and lowering the temperature continuously over 15 minutes.The gas addition lance was removed.

[0257] The reactor temperature was cooled by lowering the inductionfurnace power to 1 kW or less as the ingot cooled. The tin/lead/zincalloy was then cooled to approximately ambient temperature in water.

ANALYTICAL PROTOCOLS

[0258] XRF, grain size, magnetism, and chemical reactivity measurementswere carried out by the procedures described in Example 1.

ANALYTICAL RESULTS

[0259] An x-ray fluorescence analysis of the tinAead/zinc alloy sampleis provided in FIG. 38, with the K_(α) peak of a tin control standardshown for reference.

[0260] An x-ray fluorescence analysis of the tinflead/zinc alloy sampleis provided in FIG. 39, with the K_(α) peak of a zinc control standardshown for reference.

[0261] An x-ray fluorescence analysis of the tin/lead/zinc alloy sampleis provided in FIG. 40, with the K_(α) peak of a lead control standardshown for reference.

[0262] Summary data showing the apparent elemental composition of theproduct of Example 5 is shown in Tables 20-21, as was measured by an XRFanalysis using a Uniquant software package. The apparent elementalcomposition of the product varies by position, which is indicated ineach table.

[0263] The manufactured tin-based alloy exhibited some stratificationalong the sides of the ingot. The top (axial) face and the side (radial)face did not appear significantly different in coloration or appearance,and each had a matte finish. Like other manufactured alloy ingot,apparent peaks were exhibited on the axial face of the ingot.

[0264] The ingot did not have an internal void. No unexpected chemicalactivity or magnetic activity were recorded. The ingot did not crackupon retrieval from the reactor and retained a small amount ofrefractory.

EXAMPLE 6 Experimental Procedure for Tin/Sodium, Magnesium and Potassium14-01-08

[0265] A cylindrical alumina-based crucible (99.68% Al₂O₃, 0.07% SiO₂,0.08% Fe₂O₃, 0.04% CaO, 0.12% Na₂O₃; 4.5″ O.D.×3.75″ I.D.×10″ depth) ofa 100 pound induction furnace reactor supplied by Inductotherm andfitted with a 75-30 R Powertrak power supply, was charged with 2000 gtin (99.9% purity), plus 50 g each of sodium (99.8% pure), potassium(98% pure) and magnesium (99.98% pure) through its charging port. Thereactor was fitted with a graphite cap with a ceramic liner (i.e. thecrucible, from Engineering Ceramics). During the entire procedure, aslight positive pressure of nitrogen (˜0.5 psi) was maintained in thereactor using a continuous backspace purge. The reactor was heated tothe metal charge liquidus point plus 300° F., at a rate no greater than300° F./hour, as limited by the integrity of the crucible. The inductionfurnace operated in the frequency range of 0 kHz to 3000 kHz, withfrequency determined by a temperature-controlled feedback loopimplementing an Omega Model CN300 temperature controller. Upon reaching900° F., the reactor was charged with an additional 2120 g Sn over anhour.

[0266] The temperature was again increased to 932° F. again using a rateno greater than 300° F./hour. When this temperature was reached,graphite saturation assemblies (⅜″ OD, 36″ long high purity (<5 ppmimpurities) graphite rods) were inserted to the bottom of the Sn/Na/K/Mgcharge through ports located in the top plate. The Sn/Na/K/Mg alloy washeld at 932° F. for 4 hours. Every 30 minutes during the hold period, anattempt was made to lower the graphite saturation assemblies asdissolution occurred. As the Sn/Na/K/Mg alloy became saturated withcarbon, the graphite saturation assemblies were consumed. After the 4hour hold period was complete, the graphite saturation assemblies wereremoved.

[0267] The reactor temperature was increased to 968° F. over 7 minutes.The temperature was then varied between 942° F. and 968° F. for 15cycles. Each cycle consisted of lowering the temperature continuouslyover 7 minutes and raising the temperature continuously over 7 minutes.After the 15 cycles were completed, a gas addition lance was loweredinto the molten metal to a position approximately 2″ from the bottom ofthe reactor and a 0.15 L/min flow of argon was begun. The temperature ofthe Sn/Na/K/Mg alloy was varied over another 5 cycles between 942° F.and 968° F.

[0268] After the fifth cycle, the reactor temperature was lowered to932° F. over a 10 minute period with continued argon addition. Thegraphite saturation assemblies were reinstalled in thetin/sodium/potassium/magnesium alloy and remained there for 1 hour. Thegraphite saturation assemblies were removed.

[0269] The reactor temperature was lowered to 930° F. over 5 minutes.The reactor was held at this temperature for 5 minutes with continuedargon addition. The temperature was then varied between 918° F. and 930°F. over 20 cycles. Each cycle consisted of lowering the temperaturecontinuously over 9 minutes and raising the temperature continuouslyover 9 minutes. The argon addition ceased after completion of the 20cycles.

[0270] The reactor temperature was lowered to 924° F. over 5 minutes.The temperature was varied between 918° F. and 924° F. over 4½ cycles.Each cycle consisted of lowering the temperature continuously over 5minutes and raising the temperature continuously over 3 minutes. Inaddition, while raising the temperature, a 0.15 L/min flow of argon wasadded, and while lowering the temperature, a 0.15 L/min flow of nitrogenwas added.

[0271] The reactor temperature was lowered to 916° F. over 5 minutes.The temperature was varied between 894° F. and 916° F. for 15.5 cycles.Each cycle consisted of lowering the temperature continuously over 15minutes and raising the temperature continuously over 15 minutes. Inaddition, while raising the temperature, a 0.15 L/min flow of argon wasadded, and while lowering the temperature, a 0.15 L/min flow of nitrogenwas added. All gas addition, except for the purge of nitrogen ceasedafter the 15.5 cycles were completed.

[0272] The temperature was varied between 894° F. and 903° F. for onecycle. The cycle consisted of raising the temperature continuously over15 minutes and lowering the temperature continuously over 15 minutes.The gas addition lance was removed.

[0273] The reactor temperature was cooled by lowering the inductionfurnace power to 1 kW or less as the ingot cooled. Thetin/sodium/magnesium/potassium alloy solidified into an ingot. Aftersolidification, the alloy was cooled to approximately ambienttemperature in water.

ANALYTICAL PROTOCOLS

[0274] XRF, grain size, magnetism, and chemical reactivity measurementswere carried out by the procedures described in Example 1.

ANALYTICAL RESULTS

[0275] An x-ray fluorescence analysis of thetin/sodium/potassium/magnesium alloy sample is provided in FIG. 41, withthe K_(α) peak of a potassium (from potassium chloride) control standardshown for reference.

[0276] An x-ray fluorescence analysis of thetin/sodium/potassium/magnesium alloy sample is provided in FIG. 42, withthe K_(α) peak of a tin control standard shown for reference.

[0277] An x-ray fluorescence analysis of thetin/sodium/potassium/magnesium alloy sample is provided in FIG. 43, withthe K_(α) peak of a magnesium control standard shown for reference.

[0278] An x-ray fluorescence analysis of thetin/sodium/potassium/magnesium alloy sample is provided in FIG. 44, withthe K_(α) peak of a sodium (from AlNa₃F₆) control standard shown forreference.

[0279] Summary data showing the apparent elemental composition of theproduct of Example 6 is shown in Tables 22-23, as was measured by an XRFanalysis using a Uniquant software package. The apparent elementalcomposition of the product varies by position, which is indicated ineach table.

[0280] The ingot had a uniform dull matte finish on axial and radialsurfaces (i.e., isotropic coloration). Minimal refractory was retainedupon retrieval from the reactor. No internal voids were found in theingot. No unexpected magnetic or chemical activity were observed.

EXAMPLE 7 Experimental Procedure for Silicon 15-01-01

[0281] A cylindrical alumina-based crucible (99.68% Al₂O₃, 0.07% SiO₂,0.08% Fe₂O₃, 0.04% CaO, 0.12% Na₂O₃; 4.5″ O.D.×3.75″ I.D.×10″ depth) ofa 100 pound induction furnace reactor (Inductotherm) fitted with a 75-30R Powertrak power supply was charged with 700 g Silicon (100.00%purity), through its charging port. The reactor was fitted with agraphite cap and a ceramic liner (i.e., the crucible, from EngineeringCeramics). During the entire procedure, a slight positive pressure ofnitrogen (˜0.5 psi) was maintained in the reactor using a continuousbackspace purge. The reactor was heated to the metal charge liquiduspoint plus 300° F., at a rate no greater than 300° F./hour as limited bythe integrity of the crucible. The induction furnace operated in thefrequency range of 0 kHZ to 3000kHz, with frequency determined by atemperature-controlled feedback loop implementing an Omega Model CN 300temperature controller. Upon reaching 2800° F., the reactor was chargedwith an additional 400 g Silicon again using a rate no greater than 300°F./hour.

[0282] The temperature was again increased to 2900° F. again using arate no greater than 300° F./hour. When this temperature was reached,graphite saturation assemblies (⅜″ OD, 36″ long high purity (5 ppmimpurities) graphite rods) were inserted to the bottom of the Siliconcharge through ports located in the top plate. The Silicon was held at2900° F. for 4 hours. Every 30 minutes during the hold period, anattempt was made to lower the graphite saturation assemblies asdissolution occurred. As the Silicon became saturated with carbon, thegraphite saturation assemblies were consumed. After the 4 hour holdperiod was complete, the graphite saturation assemblies were removed.

[0283] The reactor temperature was increased to 2976° F. over 7 minutes.The temperature was then varied between 2920° F. and 2976° F. for 15cycles. Each cycle consisted of lowering the temperature continuouslyover 7 minutes and raising the temperature continuously over 7 minutes.After the 15 cycles were completed, a gas addition lance was loweredinto the molten metal to a position approximately 2″ from the bottom ofthe reactor and a 0.15 L/min flow of argon was begun. The temperature ofthe Silicon was varied over another 5 cycles between 2920° F. and 2976°F.

[0284] After the fifth cycle, the reactor temperature was lowered to2900° F. over a 10 minute period with continued argon addition. Thegraphite saturation assemblies were reinstalled in the Silicon andremained there for 1 hour. The graphite saturation assemblies wereremoved.

[0285] The reactor temperature was lowered to 2895° F. over 5 minutes.The reactor was held at this temperature for 5 minutes with continuedargon addition. The temperature was then varied between 2886° F. and2895° F. over 20 cycles. Each cycle consisted of lowering thetemperature continuously over 9 minutes and raising the temperaturecontinuously over 9 minutes. The argon addition ceased after completionof the 20 cycles.

[0286] The reactor temperature was lowered to 2873° F. over 5 minutes.The temperature was varied between 2868° F. and 2873° F. over 4½ cycles.Each cycle consisted of lowering the temperature continuously over 5minutes and raising the temperature continuously over 3 minutes. Inaddition, while raising the temperature, a 0.15 L/min flow of argon wasadded, and while lowering the temperature, a 0.15 L/min flow of nitrogenwas added.

[0287] The reactor temperature was lowered to 2863° F. over 5 minutes.The temperature was varied between 281 1° F. and 2863° F. for 15.5cycles. Each cycle consisted of lowering the temperature continuouslyover 15 minutes and raising the temperature continuously over 15minutes. In addition, while raising the temperature, a 0.15 Umin flow ofargon was added, and while lowering the temperature, a 0.15 L/min flowof nitrogen was added. All gas addition, except for the purge ofnitrogen ceased after the 15.5 cycles were completed.

[0288] The temperature was varied between 2833° F. and 2811° F. for onecycle. The cycle consisted of raising the temperature continuously over15 minutes and lowering the temperature continuously over 15 minutes.The gas addition lance was removed.

[0289] The reactor temperature was slowly cooled by lowering theinduction furnace power to 1 kW or less s the ingot cooled. Aftersolidification, the Silicon was cooled to approximately ambienttemperature in water.

ANALYTICAL PROTOCOLS

[0290] XRF, grain size, magnetism, and chemical reactivity measurementswere carried out by the procedures described in Example 1.

ANALYTICAL RESULTS

[0291] An x-ray fluorescence analysis of the silicon sample is providedin FIGS. 45A and 45B, with the K_(α) and L_(α) peaks of a siliconcontrol standard shown for reference.

[0292] An x-ray fluorescence analysis of the silicon sample is providedin FIG. 46A, with the K_(α) peak of an aluminum control standard shownfor reference.

[0293] An x-ray fluorescence analysis of the silicon sample is providedin FIG. 46B, with the K_(α) peak of a titanium control standard shownfor reference.

[0294] An x-ray fluorescence analysis of the silicon sample is providedin FIG. 47A, with the K_(α) peak of a sulfur control standard shown forreference.

[0295] An x-ray fluorescence analysis of the silicon sample is providedin FIG. 47B, with the K_(α) peak of a chlorine (from potassium chloride)control standard shown for reference.

[0296] An x-ray fluorescence analysis of the silicon sample is providedin FIG. 48A, with the K_(α) peak of a gallium control standard shown forreference.

[0297] An x-ray fluorescence analysis of the silicon sample is providedin FIG. 48B, with the K_(α) peak of a potassium control standard shownfor reference.

[0298] Summary data showing the apparent elemental composition of theproduct of Example 7 is shown in Tables 24-27, as was measured by an XkFanalysis using a Uniquant software package. The apparent elementalcomposition of the product varies by position, which is indicated ineach table.

[0299] No unexpected magnetic activity or chemical reactivity wererecorded for the ingot. The manufactured silicon system did appear shinyon its axial (top) face and dull on is radial (side) face. The ingotretained minimal refractory upon removal from the reactor.

EXAMPLE 8 Experimental Procedure for Iron 15-01-02

[0300] A cylindrical alumina-based crucible (99.68% Al₂O₃, 0.07% SiO₂,0.08% Fe₂O₃, 0.04% CaO, 0.12% Na₂O₃; 4.5″ O.D.×3.75″ I.D.×10″ depth) ofa 100 pound induction furnace reactor supplied by Inductotherm, fittedwith a 75-30 R Powertrak power supply was charged with 2000 g Iron(99.98% purity) and 200 g carbon through its charging port. The reactorwas fitted with a graphite cap with a ceramic liner (i.e. the crucible,from Engineering Ceramics). During the entire procedure, a slightpositive pressure of nitrogen (˜0.5 psi) was maintained in the reactorusing a continuous backspace purge. The reactor was heated to the metalcharge liquidus point plus 300° F., at a rate no greater than 300°F./hour, as limited by the integrity of the crucible. The inductionfurnace operated in the frequency range of 0 kHz to 3000 kHz, withfrequency determined by a temperature-controlled feedback loopimplementing an Omega Model CN300 temperature controller. Upon reaching2800° F., the reactor was charged with an additional 2595 g iron over anhour.

[0301] The temperature was again increased to 2850° F. again using arate no greater than 300° F./hour. When this temperature was reached,graphite saturation assemblies (⅜ OD, 36″ long high purity (<5ppmimpurities) graphite rods) were inserted to the bottom of the ironcharge through ports located in the top plate. The iron was held at2850° F. for 4 hours. Every 30 minutes during the hold period, anattempt was made to lower the graphite saturation assemblies asdissolution occurred. As the iron became saturated with carbon, thegraphite saturation assemblies were consumed. After the 4 hour holdperiod was complete, the graphite saturation assemblies were removed.

[0302] The reactor temperature was increased to 3360° F. over 7 minutes.The temperature was then varied between 2993° F. and 3360° F. for 15cycles. Each cycle consisted of lowering the temperature continuouslyover 7 minutes and raising the temperature continuously over 7 minutes.After the 15 cycles were completed, a gas addition lance was loweredinto the molten metal to a position approximately 2″ from the bottom ofthe reactor and a 0.15 L/min flow of argon was begun. The temperature ofthe iron was varied over another 5 cycles between 2993° F. and 3360° F.

[0303] After the fifth cycle, the reactor temperature was lowered to2850° F. over,a 10 minute period with continued argon addition. Thegraphite saturation assemblies were reinstalled in the iron and remainedthere for 1 hour. The graphite saturation assemblies were removed.

[0304] The reactor temperature was lowered to 2819° F. over 5 minutes.The reactor was held at this temperature for 5 minutes with continuedargon addition. The temperature was then varied between 2622° F. and2818° F. over 20 cycles. Each cycle consisted of lowering thetemperature continuously over 9 minutes and raising the temperaturecontinuously over 9 minutes. The argon addition ceased after completionof the 20 cycles.

[0305] The reactor temperature was lowered to 2724° F. over 5 minutes.The temperature was varied between 2622° F. and 2724° F. over 4½ cycles.Each cycle consisted of lowering the temperature continuously over 5minutes and raising the temperature continuously over 3 minutes. Inaddition, while raising the temperature, a 0.15 L/min flow of argon wasadded, and while lowering the temperature, a 0.15 L/min flow of nitrogenwas added.

[0306] The reactor temperature was lowered to 2586° F. over 5 minutes.The temperature was varied between 2133° F. and 2586° F. for 15.5cycles. Each cycle consisted of lowering the temperature continuouslyover 15 minutes and raising the temperature continuously over 15minutes. In addition, while raising the temperature, a 0.15 L/min flowof argon was added, and while lowering the temperature, a 0.15 L/minflow of nitrogen was added. All gas addition, except for the purge ofnitrogen ceased after the 15.5 cycles were completed.

[0307] The temperature was varied between 2340° F. and 2133° F. for onecycle. The cycle consisted of raising the temperature continuously over15 minutes and lowering the temperature continuously over 15 minutes.The gas addition lance was removed.

[0308] The reactor temperature was cooled by lowering the inductionfurnace power to 1 kW or less as the ingot cooled. After solidification,the iron was cooled to approximately ambient temperature in water.

ANALYTICAL PROTOCOLS

[0309] XRF, grain size, magnetism, and chemical reactivity measurementswere carried out by the procedures described in Example 1.

ANALYTICAL RESULTS

[0310] An x-ray fluorescence analysis of the iron sample is provided inFIGS. 49A and 49B, with the K_(α) and L_(α) peaks of an iron controlstandard shown for reference.

[0311] An x-ray fluorescence analysis of the iron sample is provided inFIG. 50A, with the K_(α) peak of an aluminum control standard shown forreference.

[0312] An x-ray fluorescence analysis of the iron sample is provided inFIG. 50B, with the K_(α) peak of an zirconium control standard shown forreference.

[0313] An x-ray fluorescence analysis of the iron sample is provided inFIG. 51A, with the K_(α) peak of a sulfur control standard shown forreference.

[0314] An x-ray fluorescence analysis of the iron sample is provided inFIG. 51B, with the K_(α) peak of a chlorine (from potassium chloride)control standard shown for reference.

[0315] Summary data showing the apparent elemental composition of theproduct of Example 8 is shown in Tables 28-29, as was measured by an XRFanalysis using a Uniquant software package. The apparent elementalcomposition of the product varies by position, which is indicated ineach table.

[0316] The manufactured iron exhibited no unexpected magnetic activity.The reactivity relative to that which would be expected from naturaliron has not been quantified. The ingot appears glassy or shiny on itsaxial (top) face and dull on its radial (side) face. The manufacturediron retained a negligible amount of refractory upon removal from thereactor, but cracked upon retrieval. The in got had no internal voids.

EXAMPLE 9 Experimental Procedure for Iron W/Vandium, Chromium andManganese 15-01-03

[0317] A cylindrical alumina-based crucible (99.68% Al₂O₃, 0.07% SiO₂,0.08% Fe₂O₃, 0.04% CaO, 0.12% Na₂O₃; 4.5″ O.D.×3.75″ I.D.×10″ depth) ofa 100 pound induction furnace reactor supplied by Inductotherm, fittedwith a 75-30R Powertrak power supply, was charged with 2000 g Iron(99.98% purity), plus 91.9 g each of Vanadium (99.5% pure), Chromium(99% pure), and Manganese (99.9% pure), plus 200 g of carbon through itscharging port. The reactor was fitted with a graphite cap with a ceramicliner (i.e., the crucible, from Engineering Ceramics). During the entireprocedure, a slight positive pressure of nitrogen (˜0.5 psi) wasmaintained in the reactor using a continuous backspace purge. Thereactor was heated to the metal charge liquidus point plus 300° F., at arate no greater than 300° F./hour as limited by the integrity of thecrucible. The inductionfurnace operated in the frequency range of 0 kHzto 3000 kHz, with frequency determined by a temperature-controlledfeedback loop implementing an Omega Model CN300 temperature controller.Upon reaching 2800° F., the reactor was charged with an additional2319.3 g iron over an hour.

[0318] The temperature was again increased to 2850° F. again using arate no greater than 300° F./hour. When this temperature was reached,graphite saturation assemblies (⅜″ OD, 36″ long high purity graphiterods) were inserted to the bottom of the metal charge through portslocated in the top plate . The alloy was held at 2850° F. for 4 hours.Every 30 minutes during the hold period, an attempt was made to lowerthe graphite saturation assemblies as dissolution occurred. As the alloybecame saturated with carbon, the graphite saturation assemblies wereconsumed. After the 4 hour hold period was complete, the graphitesaturation assemblies were removed.

[0319] The reactor temperature was increased to 3360° F. over 7 minutes.The temperature was then varied between 2993° F. and 3360° F. for 15cycles. Each cycle consisted of lowering the temperature continuouslyover 7 minutes and raising the temperature continuously over 7 minutes.After the 15 cycles were completed, a gas addition lance was loweredinto the molten metal to a position approximately 2″ from the bottom ofthe reactor and a 0.15 L/min flow of argon was begun. The temperature ofthe iron was varied over another 5 cycles between 2993° F. and 3360° F.

[0320] After the fifth cycle, the reactor temperature was lowered to2850° F. over a 10 minute period with continued argon addition. Thegraphite saturation assemblies were reinstalled in the iron and remainedthere for 1 hour. The graphite saturation assemblies were removed.

[0321] The reactor temperature was lowered to 2819° F. over 5 minutes.The reactor was held at this temperature for 5 minutes with continuedargon addition. The temperature was then varied between 2622° F. and2818° F. over 20 cycles. Each cycle consisted of lowering thetemperature continuously over 9 minutes and raising the temperaturecontinuously over 9 minutes. The argon addition ceased after completionof the 20 cycles.

[0322] The reactor temperature was lowered to 2724° F. over 5 minutes.The temperature was varied between 2622° F. and 2724° F. over 4½ cycles.Each cycle consisted of lowering the temperature continuously over 5minutes and raising the temperature continuously over 3 minutes. Inaddition, while raising the temperature, a 0.15 L/min flow of argon wasadded, and while lowering the temperature, a 0.15 L/min flow of nitrogenwas added.

[0323] The reactor temperature was lowered to 2586° F. over 5 minutes.The temperature was varied between 2133° F. and 2586° F. for 15.5cycles. Each cycle consisted of lowering. the temperature continuouslyover 15 minutes and raising the temperature continuously over 15minutes. In addition, while raising the temperature, a 0.15 L/min flowof argon was added, and while lowering the temperature, a 0.15 L/minflow of nitrogen was added. All gas addition, except for the purge ofnitrogen ceased after the 15.5 cycles were completed.

[0324] The temperature was varied between 2340° F. and 2133° F. for onecycle. The cycle consisted of raising the temperature continuously over15 minutes and lowering the temperature continuously over 15 minutes.The gas addition lance was removed.

[0325] The reactor temperature was cooled by lowering the inductionfurnace power to 1 kW or less as the ingot cooled. Theiron/vanadium/chromium/manganese alloy was the cooled to approximatelyambient temperature in water.

ANALYTICAL PROTOCOLS

[0326] XRF, grain size, magnetism, and chemical reactivity measurementswere carried out by the procedures described in Example 1.

ANALYTICAL RESULTS

[0327] An x-ray fluorescence analysis of theiron/vanadium/chromium/manganese alloy sample is provided in FIG. 52,with the K_(α) peak of a chromium (from chromium(III) oxide) controlstandard shown for reference.

[0328] An x-ray fluorescence analysis of theiron/vanadium/chromium/manganese alloy sample is provided in FIG. 53,with the K_(α) peak of an iron control standard shown for reference.

[0329] An x-ray fluorescence analysis of theiron/vanadium/chromium/manganese alloy sample is provided in FIG. 54,with the K_(α) peak of a vanadium control standard shown for reference.

[0330] An x-ray fluorescence analysis of theiron/vanadium/chromium/manganese alloy sample is provided in FIG. 55,with the K_(α) peak of a manganese control standard shown for reference.

[0331] An x-ray fluorescence analysis of theiron/vanadium/chromium/manganese alloy sample is provided in FIG. 56, inthe region of the K_(α) peak of a sulfur control standard.

[0332] Summary data showing the apparent elemental composition of theproduct of Example 9 is shown in Tables 40-41, as was measured by an XRFanalysis using a Uniquant software package. The apparent elementalcomposition of the product varies by position, which is indicated ineach table.

[0333] Upon polishing the manufactured alloy in preparation for XRFanalysis, the alloy was noted to be particularly hard and astratification pattern that was not attributable to the polishingmaterials was exposed. The relative hardness of the alloy was tested andthe Moh's hardness was found to be greater than what would be expectedfrom a natural alloy of a similar composition. The radial surface of theingot had a shiny or glassy appearance, while the axial surface appeareddull, thus reflecting bulk anisotropic behavior.

[0334] The manufactured alloy had no unexpected magnetic activity. Theingot retained a negligible amount of refractory upon retrieval from thereactor, but did crack.

EXAMPLE 10 Experimental Procedure for Nickel W/Tantalum Hafnium andTungsten 15-01-04

[0335] A cylindrical alumina-based crucible (99.68% Al₂O₃, 0.07% SiO₂,0.08% Fe₂O₃, 0.04% CaO, 0.12% Na₂O₃; 4.5″ O.D.×3.75″ I.D.×10″ depth) ofa 100 pound induction furnace reactor supplied by Inductotherm, fittedwith a 75-30R Powertrak power supply and was charged with 2500 g Nickel(99.9% purity), plus 100 g each of Hafnium (99.9% pure), W (99.9% pure),Ta (99.98% pure), and carbon through its charging port. The reactor wasfitted with a graphite cap with a ceramic liner (i.e., the crucible,from Engineering Ceramics). During the entire procedure, a slightpositive pressure of nitrogen (˜0.5 psi) was maintained in the reactorusing a continuous backspace purge. The reactor was heated to the metalcharge liquidus point plus 300° F., at a rate no greater than 300°F./hour, as limited by the integrity of the crucible. The inductionfurnace operated in the frequency range of 0 kHz to 3000 kHz, withfrequency determined by a temperature-controlled feedback loopimplementing an Omega Model CN300 temperature controller. Upon reaching2800° F., the reactor was charged with an additional 2200 g nickel overan hour.

[0336] The temperature was again increased to 2850° F. again using arate no greater than 300° F./hour. When this temperature was reached,graphite saturation assemblies (⅜″ OD, 36″ long high purity (<5 ppmimpurities) graphite rods) were inserted to the bottom of the metalcharge through ports located in the top plate. The alloy was held at2850° F. for 4 hours. Every 30 minutes during the hold period, anattempt was made to lower the graphite saturation assemblies asdissolution occurred. As the alloy became saturated with carbon, thegraphite saturation assemblies were consumed. After the 4 hour holdperiod was complete, the graphite saturation assemblies were removed.

[0337] The reactor temperature was increased to 3256° F. over 7 minutes.The temperature was then varied between 2950° F. and 3256° F. for 15cycles. Each cycle consisted of lowering the temperature continuouslyover 7 minutes and raising the temperature continuously over 7 minutes.After the 15 cycles were completed, a gas addition lance was loweredinto the molten metal to a position approximately 2″ from the bottom ofthe reactor and a 0.15 L/min flow of argon was begun. The temperature ofthe alloy was varied over another 5 cycles between 2950° F. and 3256° F.

[0338] After the fifth cycle, the reactor temperature was lowered to2850° F. over a 10 minute period with continued argon addition. Thegraphite saturation assemblies were reinstalled in the alloy andremained there for 1 hour. The graphite saturation assemblies wereremoved.

[0339] The reactor temperature was lowered to 2829° F. over 5 minutes.The reactor was held at this temperature for 5 minutes with continuedargon addition. The temperature was then varied between 2790° F. and2829OF over 20 cycles. Each cycle consisted of lowering the temperaturecontinuously over 9 minutes and raising the temperature continuouslyover 9 minutes. The argon addition ceased after completion of the 20cycles.

[0340] The reactor temperature was lowered to 2770° F. over 5 minutes.The temperature was varied between 2710° F. and 2770° F. over 4½ cycles.Each cycle consisted of lowering the temperature continuously over 5minutes and raising the temperature continuously over 3 minutes. Inaddition, while raising the temperature, a 0.15 L/min flow of argon wasadded, and while lowering the temperature, a 0.15 L/min flow of nitrogenwas added.

[0341] The reactor temperature was lowered to 2691° F. over 5 minutes.The temperature was varied between 2492° F. and 2691° F. for 15.5cycles. Each cycle consisted of lowering the temperature continuouslyover 15 minutes and raising the temperature continuously over 15minutes. In addition, while raising the temperature, a 0.15 L/min flowof argon was added, and while lowering the temperature, a 0.15 L/minflow of nitrogen was added. All gas addition, except for the purge ofnitrogen ceased after the 15.5 cycles were completed.

[0342] The temperature was varied between 2571° F. and 2492° F. for onecycle. The cycle consisted of raising the temperature continuously over15 minutes and lowering the temperature continuously over 15 minutes.The gas addition lance was removed.

[0343] The reactor temperature was slowly cooled by lowering theinduction furnace power to 1 kW or less as the ingot cooled. Aftersolidification, the alloy was cooled to approximately ambienttemperature in water.

ANALYTICAL PROTOCOLS

[0344] XRF, grain size, magnetism, and chemical reactivity measurementswere carried out by the procedures described in Example 1.

ANALYTICAL RESULTS

[0345] An x-ray fluorescence analysis of thenickel/hafnium/tantalum/tungsten alloy sample is provided in FIG. 57,with the K_(α) peak of a tantalum control standard shown for reference.

[0346] An x-ray fluorescence analysis of thenickel/hafniurn/tantalum/tungsten alloy sample is provided in FIG. 58,with the K_(α) peak of a tungsten control standard shown for reference.

[0347] An x-ray fluorescence analysis of thenickel/hafnium/tantalum/tungsten alloy sample is provided in FIG. 59,with the K_(α) peak of a hafnium control standard shown for reference.

[0348] An x-ray fluorescence analysis of thenickel/hafnium/tantalum/tungsten alloy sample is provided in FIG. 60, inthe region of the K_(α) peak of a sulfur control standard.

[0349] An x-ray fluorescence analysis of thenickel/hafnium/tantalum/tungsten alloy sample is provided in FIG. 61,with the K_(α) peak of a nickel control standard shown for reference.

[0350] Summary data showing the apparent elemental composition of theproduct of Example 10 is shown in Tables 30-31, as was measured by anXRF analysis using a Uniquant software package. The apparent elementalcomposition of the product varies by position, which is indicated ineach table.

[0351] The manufactured nickel-based alloy exhibited clear anisotropicbehavior with respect to color and reactivity similar to the anisotropyobserved via XRF. The sides were covered with a large amount ofrefractory retained after the ingot was retrieved from the reactor. Thetop face had a classic metallic sheen. No unexpected magnetic activitywas observed. The ingot did not upon removal from the reactor or exhibitany internal voids.

EXAMPLE 11 Experimental Procedure for Copper 14-00-01

[0352] A cylindrical alumina-based crucible (89.07% Al₂O₃, 10.37% SiO₂,0.16% TiO₂, 0.15% Fe₂O₃, 0.03% CaO, 0.01% MgO, 0.02% Na₂O₃, 0.02% K₂O;9O.D.×7.75″ I.D.×14″ depth) of a 100 pound induction furnace reactorsupplied by Inductotherm, fitted with a 75-30 R Powertrak power supply,was charged with 100 pounds copper (99.98% purity) through its chargingport. During the entire procedure, a slight positive pressure ofnitrogen (˜0.5 psi) was maintained in the reactor using a continuousbackspace purge. The reactor was heated to the metal charge liquiduspoint plus 300° F., at a rate no greater than 300° F./hour, as limitedby the integrity of the crucible. The induction furnace operated in thefrequence range of 0 kHz to 3000 kHz, with frequency determined by atemperature-controlled feedback loop implementing an Omega Model CN300temperature controller.

[0353] The temperature was again increased to 2462° F. again using arate no greater than 300° F./hour. When this temperature was reached,graphite saturation assemblies (⅜″ OD, 36″ long high purity (<5 ppmimpurities) graphite rods) were inserted to the bottom of the coppercharge through ports located in the top plate. The copper was held at2462° F. for 4 hours. Every 30 minutes during the hold period, anattempt was made to lower the graphite saturation assemblies asdissolution occurred. As the copper became saturated with carbon, thegraphite saturation assemblies were consumed. After the 4 hour holdperiod was complete, the graphite saturation assemblies were removed.

[0354] The reactor temperature was increased to 2480° F. over 7 minutes.The temperature was then varied between 2480° F. and 2530° F. for 15cycles. Each cycle consisted of raising the temperature continuouslyover 7 minutes and lowering the temperature continuously over 7 minutes.After the 15 cycles were completed, a gas addition lance was loweredinto the molten metal to a position approximately 2″ from the bottom ofthe reactor and a 1.5 L/min flow of argon was begun. The temperature ofthe copper was varied over another 5 cycles between 2480° F. and 2530°F.

[0355] After the fifth cycle, the reactor temperature was lowered to2462° F. over a 10 minute period with continued argon addition. Thegraphite saturation assemblies were reinstalled in the copper andremained there for 1 hour. The graphite saturation assemblies wereremoved.

[0356] The reactor temperature was lowered to 2459° F. over 5 minutes.The reactor was held at this temperature for 5 minutes with continuedargon addition. The temperature was then varied between 2459° F. and2453° F. over 20 cycles. Each cycle consisted of lowering thetemperature continuously over 9 minutes and raising the temperaturecontinuously over 9 minutes. The argon addition ceased after completionof the 20 cycles.

[0357] The reactor temperature was lowered to 2450° F. over 5 minutes.The temperature was varied between 2450° F. and 2441° F. over 4½ cycles.Each cycle consisted of lowering the temperature continuously over 5minutes and raising the temperature continuously over 3 minutes. Inaddition, while raising the temperature, a 1.5 L/min flow of argon wasadded, and while lowering the temperature, a 1.5 L/min flow of nitrogenwas added.

[0358] The reactor temperature was lowered to 2438° F. over 5 minutes.The temperature was varied between 2438° F. and 2406° F. for 15.5cycles. Each cycle consisted of lowering the temperature continuouslyover 15 minutes and raising the temperature continuously over 15minutes. In addition, while raising the temperature, a 1.5 L/min flow ofargon was added, and while lowering the temperature, a 1.5 L/min flow ofnitrogen was added. All gas addition, except for the purge of nitrogenceased after the 15.5 cycles were completed.

[0359] The temperature was varied between 2406° F. and 2419° F. for onecycle. The cycle consisted of raising the temperature continuously over15 minutes and lowering the temperature continuously over 15 minutes.The gas addition lance was removed.

[0360] The reactor temperature was rapidly cooled by quenching in water,so that the copper solidified into an ingot.

ANALYTICAL PROTOCOLS

[0361] XRF, grain size, magnetism, and chemical reactivity measurementswere carried out by the procedures described in Example 1.

ANALYTICAL RESULTS

[0362] Summary data showing the apparent elemental composition of the.product of Example 11 is shown in Tables 32-33, as was measured by anXRF analysis using a Uniquant software package. The apparent elementalcomposition of the product varies by position, which is indicated ineach table.

[0363] Immediately after the method described above was completed,multiple discrete magnetic spots attracted by a ⅛″ diameter neodymiumiron boron magnet were observed in a sinusoidal pattern. The ingotexhibited point attraction to iron filings at reduced temperatures at ornear 77 K. Over days to months, the strength of the magnetic attractiondecreased on a fraction of the locations exhibiting magnetic attractionor attraction to iron filings.

[0364] Various forms of ligated chlorine (e.g., HCl and MCl, where M isa metal as defined above) readily reacted with the manufactured copperform yielding product distributions distinguishable from natural copper,thereby demonstrating a change in chemical reactivity. This reactivityincreased over time.

[0365] Extremely large grain sizes (i.e., greater than 1″) wereobserved, which is uncharacteristic and previously unreported in naturalcopper systems (typically, copper grains sizes are 10-100 μm). Uniquechanges in coloration were observed with the crossing of grainboundaries; however, the overall coloration mimicked natural copper.

EXAMPLE 12 Experimental Procedure for Copper 14-00-03

[0366] A cylindrical alumina-based crucible (89.07% Al₂O₃, 10.37% SiO₂,0.16% TiO₂, 0.15% Fe₂O₃, 0.03% CaO, 0.01% MgO, 0.02% Na₂O₃, 0.02% K₂O;9″ O.D.×7.75″ I.D.×14″ depth) of a 100 pound induction furnace reactorsupplied by Inductotherm, fitted with a 75-30 R Powertrak power supplyand was charged with 100 pounds copper (99.98% purity) through itscharging port. During the entire procedure, a slight positive pressureof nitrogen (˜0.5 psi) was maintained in the reactor using a continuousbackspace purge. The reactor was heated to the metal charge liquiduspoint plus 300° F., at a rate no greater than 300° F./hour, as limitedby the integrity of the crucible. The induction furnace operated in thefrequence range of 0 kHz to 3000 kHz, with frequency determined by atemperature-controlled feedback loop implementing an Omega Model CN300temperature controller.

[0367] The temperature was again increased to 2462° F. again using arate no greater than 300° F./hour. When this temperature was reached,graphite saturation assemblies (⅜″ OD, 36″ long high purity (<5 ppmimpurities) graphite rods) were inserted to the bottom of the coppercharge through ports located in the top plate. The copper was held at2462° F. for 4 hours. Every 30 minutes during the hold period, anattempt was made to lower the graphite saturation assemblies asdissolution occurred. As the copper became saturated with carbon, thegraphite saturation assemblies were consumed. After the 4 hour holdperiod was complete, the graphite saturation assemblies were removed.

[0368] The reactor temperature was increased to 2480° F. over 7 minutes.The temperature was then varied between 2480° F. and 2530° F. for 15cycles. Each cycle consisted of raising the temperature continuouslyover 7 minutes and lowering the temperature continuously over 7 minutes.After the 15 cycles were completed, a gas addition lance was loweredinto the molten metal to a position approximately 2″ from the bottom ofthe reactor and a 1.5 L/min flow of argon was begun. The temperature ofthe copper was varied over another 5 cycles between 2480° F. and 2530°F.

[0369] After the fifth cycle, the reactor temperature was lowered to2462° F. over a 10 minute period with continued argon addition. Thegraphite saturation assemblies were reinstalled in the copper andremained there for 1 hour. The graphite saturation assemblies wereremoved.

[0370] The reactor temperature was lowered to 2459° F. over 5 minutes.The reactor was held at this temperature for 5 minutes with continuedargon addition. The temperature was then varied between 2459° F. and2453° F. over 20 cycles. Each cycle consisted of lowering thetemperature continuously over 9 minutes and raising the temperaturecontinuously over 9 minutes. The argon addition ceased after completionof the 20 cycles.

[0371] The reactor temperature was lowered to 2450° F. over 5 minutes.The temperature was varied between 2450° F. and 2441° F. over 4½ cycles.Each cycle consisted of lowering the temperature continuously over 5minutes and raising the temperature continuously over 3 minutes. Inaddition, while raising the temperature, a 1.5 L/min flow of argon wasadded, and while lowering the temperature, a 1.5 L/min flow of nitrogenwas added.

[0372] The reactor temperature was lowered to 2438° F. over 5 minutes.The temperature was varied between 2438° F. and 2406° F. for 15.5cycles. Each cycle consisted of lowering the temperature continuouslyover 15 minutes and raising the temperature continuously over 15minutes. In addition, while raising the temperature, a 1.5 L/min flow ofargon was added, and while lowering the temperature, a 1.5 L/min flow ofnitrogen was added. All gas addition, except for the purge of nitrogenceased after the 15.5 cycles were completed.

[0373] The temperature was varied between 2406° F. and 2419° F. for onecycle. The cycle consisted of raising the temperature continuously over15 minutes and lowering the temperature continuously over 15 minutes.The gas addition lance was removed.

[0374] The reactor temperature was rapidly cooled by quenching in water,so that the copper solidified into an ingot.

ANALYTICAL PROTOCOLS

[0375] XRF, grain size, magnetism, and chemical reactivity measurementswere carried out by the procedures described in Example 1.

ANALYTICAL RESULTS

[0376] Summary data showing the apparent elemental composition of theproduct of Example 12 is shown in Tables 34-35, as was measured by anXRF analysis using a Uniquant software package. The apparent elementalcomposition of the product varies by position, which is indicated ineach table.

[0377] This manufactured copper system demonstrated an ability to changecolor (i.e., visible light spectrum emission) dependent uponelectromagnetic stimulation. The color of the top, glassy surface of aningot changed under different lighting conditions. While the (radial)side of the ingot was a matte pink color, the top of the ingot (axialface) has a glassy color, which can vary from intense burgundy to goldenbronze to burnished orange. These differences in appearance-reflect theanisotropy detected via the XRFs.

[0378] The radial surface of the ingot was covered with magneticallyactive spots. The magnetism of the ingot decreased over time. Alteredchemical reactivity, particularly with respect to ligated chlorine, wasobserved on axial surfaces. The chemical reactivity increased over time.Radial surfaces appeared unaffected and were free from refractory(material from the crucible).

EXAMPLE 13 Experimental Procedure for Copper 14-00-04

[0379] A cylindrical alumina-based crucible (89.07% Al₂O₃, 10.37% SiO₂,0.16% TiO₂, 0.15% Fe₂O₃, 0.03% CaO, 0.01% MgO, 0.02% Na₂O₃, 0.02% K₂O;9″ O.D.×7.75″ I.D.×14″ depth) of a 100 pound induction fuimace reactorsupplied by Inductotherm, fitted with a 75-30 R Powertrak power supplywas charged with 100 pounds copper (99.98% purity) through its chargingport. During the entire procedure, a slight positive pressure ofnitrogen (˜0.5 psi) was maintained in the reactor using a continuousbackspace purge. The reactor was heated to the metal charge liquiduspoint plus 300° F., at a rate no greater than 300° F./hour, as limitedby the integrity of the crucible. The induction furnace operated in thefrequence range of 0 kHz to 3000 kHz, with frequency determined by atemperature-controlled feedback, loop implementing an Omega Model CN300temperature controller

[0380] The temperature was again increased to 2462° F. again using arate no greater than 300° F./hour. When this temperature was reached,graphite saturation assemblies (⅜″ OD, 36″ long high purity (<5 ppmimpurities) graphite rods) were inserted to the bottom of the coppercharge through ports located in the top plate. The copper was held at2462° F. for 4 hours. Every 30 minutes during the hold period, anattempt was made to lower the graphite saturation assemblies asdissolution occurred. As the copper became saturated with carbon, thegraphite saturation assemblies were consumed. After the 4 hour holdperiod was complete, the graphite saturation assemblies were removed.

[0381] The reactor temperature was increased to 2480° F. over 7 minutes.The temperature was then varied between 2480° F. and 2530° F. for 15cycles. Each cycle consisted of raising the temperature continuouslyover 7 minutes and lowering the temperature continuously over 7 minutes.After the 15 cycles were completed, a gas addition lance was loweredinto the molten metal to a position approximately 2″ from the bottom ofthe reactor and a 1.5 L/min flow of argon was begun The temperature ofthe copper was varied over another 5 cycles between 2480° F. and 2530°F.

[0382] After the fifth cycle, the reactor temperature was lowered to2462° F. over a 10 minute period with continued argon addition. Thegraphite saturation assemblies were reinstalled in the copper andremained there for 1 hour. The graphite saturation assemblies wereremoved.

[0383] The reactor temperature was lowered to 2459° F. over 5 minutes.The reactor was held at this temperature for 5 minutes with continuedargon addition. The temperature was then varied between 2459° F. and2453° F. over 20 cycles. Each cycle consisted of lowering thetemperature continuously over 9 minutes and raising the temperaturecontinuously over 9 minutes. The argon addition ceased after completionof the 20 cycles.

[0384] The reactor temperature was lowered to 2450° F. over 5 minutes.The temperature was varied between 2450° F. and 2441° F. over 4½ cycles.Each cycle consisted of lowering the temperature continuously over 5minutes and raising the temperature continuously over 3 minutes. Inaddition, while raising the temperature, a 1.5 L/min flow of argon wasadded, and while lowering the temperature, a 1.5 L/min flow of nitrogenwas added.

[0385] The reactor temperature was lowered to 2438° F. over 5 minutes.The temperature was varied between 2438° F. and 2406° F. for 15.5cycles. Each cycle consisted of lowering the temperature continuouslyover 15 minutes and raising the temperature continuously over 15minutes. In addition, while raising the temperature, a 1.5 L/min flow ofargon was added, and while lowering the temperature, a 1.5 L/min flow ofnitrogen was added. All gas addition, except for the purge of nitrogenceased after the 15.5 cycles were completed.

[0386] The temperature was varied between 2406° F. and 2419° F. for onecycle. The cycle consisted of raising the temperature continuously over15 minutes and lowering the temperature continuously over 15 minutes.The gas addition lance was removed.

[0387] The reactor temperature was slowly cooled and was subsequentlyquenched in water, so that the copper solidified into an ingot.

ANALYTICAL PROTOCOLS

[0388] XRF, grain size, magnetism, and chemical reactivity measurementswere carried out by the procedures described in Example 1.

ANALYTICAL RESULTS

[0389] Summary data showing the apparent elemental composition of theproduct of Example 13 is shown in Tables 36-37, as was measured by anXRF analysis using a Uniquant software package. The apparent elementalcomposition of the product varies by position, which is indicated ineach table.

[0390] The manufactured copper ingot exhibited many of thecharacteristic patterns observed in previous examples. Differences inthe coloration and appearance of the axial and radial directions wereobserved: matte, burgundy brown coloration on the side, and glassy onthe top with demarcations.

[0391] This ingot had internal voids. The ingot demonstrated enhancedchemical reactivity on the axial surfaces. Refractory was found to betightly bound to select portions of the radial surfaces. Minimalmagnetic activity was detected.

EXAMPLE 14 Experimental Procedure for Copper 15-00-01

[0392] A cylindrical alumina-based crucible (89.07% Al₂O₃, 10.37% SiO₂,0.16% TiO₂, 0.15% Fe₂O₃, 0.03% CaO, 0.01% MgO, 0.02% Na₂O₃, 0.02% K₂O;9″ O.D.×7.75″ I.D.×14″ depth) of a 100 pound induction furnace reactorsupplied by Inductotherm, fitted with a 75-30 R Powertrak power supplyand was charged with 100 pounds copper (99.98% purity) through itscharging port. During the entire procedure, a slight positive pressureof nitrogen (˜0.5 psi) was maintained in the reactor using a continuousbackspace purge. The reactor was heated to the metal charge liquiduspoint plus 300° F., at a rate no greater than 300° F./hour, as limitedby the integrity of the crucible. The induction furnace operated in thefrequence range of 0 kHz to 3000 kHz, with frequency determined by atemperature-controlled feedback loop implementing an Omega Model CN300temperature controller.

[0393] The temperature was again increased to 2462° F. again using arate no greater than 300° F./hour. When this temperature was reached,graphite saturation assemblies (⅜″ OD, 36″ long high purity (<5 ppmimpurities) graphite rods) were inserted to the bottom of the coppercharge through ports located in the top plate. The copper was held at2462° F. for 4 hours. Every 30 minutes during the hold period, anattempt was made to lower the graphite saturation assemblies asdissolution occurred. As the copper became saturated with carbon, thegraphite saturation assemblies were consumed. After the 4 hour holdperiod was complete, the graphite saturation assemblies were removed.

[0394] The reactor temperature was increased to 2480° F. over 7 minutes.The temperature was then varied between 2480° F. and 2530° F. for 15cycles. Each cycle consisted of raising the temperature continuouslyover 7 minutes and lowering the temperature continuously over 7 minutes.After the 15 cycles were completed, a gas addition lance was loweredinto the molten metal to a position approximately 2″ from the bottom ofthe reactor and a 1.5 L/min flow of argon was begun. The temperature ofthe copper was varied over another 5 cycles between 2480° F. and 2530°F.

[0395] After the fifth cycle, the reactor temperature was lowered to2462° F. over a 10 minute period with continued argon addition. Thegraphite saturation assemblies were reinstalled in the copper andremained there for 1 hour. The graphite saturation assemblies wereremoved.

[0396] The reactor temperature was lowered to 2459° F. over 5 minutes.The reactor was held at this temperature for 5 minutes with continuedargon addition. The temperature was then varied between 2459° F. and2453° F. over 20 cycles. Each cycle consisted of lowering thetemperature continuously over 9 minutes and raising the temperaturecontinuously over 9 minutes. The argon addition ceased after completionof the 20 cycles.

[0397] The reactor temperature was lowered to 2450° F. over 5 minutes.The temperature was varied between 2450° F. and 2441° F. over 4½ cycles.Each cycle consisted of lowering the temperature continuously over 5minutes and raising the temperature continuously over 3 minutes. Inaddition, while raising the temperature, a 1.5 L/min flow of argon wasadded, and while lowering the temperature, a 1.5 L/min flow of nitrogenwas added.

[0398] The reactor temperature was lowered to 2438° F. over 5 minutes.The temperature was varied between 2438° F. and 2406° F. for 15.5cycles. Each cycle consisted of lowering the temperature continuouslyover 15 minutes and raising the temperature continuously over 15minutes. In addition, while raising the temperature, a 1.5 L/min flow ofargon was added, and while lowering the temperature, a 1.5 L/min flow ofnitrogen was added. All gas addition, except for the purge of nitrogenceased after the 15.5 cycles were completed.

[0399] The temperature was varied between 2406° F. and 2419° F. for onecycle. The cycle consisted of raising the temperature continuously over15 minutes and lowering the temperature continuously over 15 minutes.The gas addition lance was removed.

[0400] The reactor temperature was slowly cooled and was subsequentlyquenched in water, so that the copper solidified into an ingot.

ANALYTICAL PROTOCOLS

[0401] XRF, grain size, magnetism, and chemical reactivity measurementswere carried out by the procedures described in Example 1.

ANALYTICAL RESULTS

[0402] Summary data showing the apparent elemental composition of theproduct of Example 14 is shown in Tables 38-39, as was measured by anXRF analysis using a Uniquant software package. The apparent elementalcomposition of the product varies by position, which is indicated ineach table.

[0403] The manufactured copper demonstrated an ability to change color(i.e., visible light spectrum emission), dependant upon electromagneticstimulation. The top (axial face) of the ingot can vary from intenseburgundy to a deep golden orange. Additionally, the appearance and colorof this ingot reflect the anisotropy detected via the XRF scans. Theradial (side) face appears like burnished copper, while the axial (top)face has a glassy appearance.

[0404] On the bottom and side faces, each of the grain boundaries isclearly delineated. Each of the grains appears to have a differentcolor, giving the exterior of the ingot an iridescent appears. The ingotdid not have an internal void, as ingots of previous examples did.Additionally, the ingot did not exhibit the extensive magnetic activityobserved in Examples 11 and 12. The ingot retained an extensive amountof refractory upon retrieval from the reactor.

[0405] While this invention has been particularly shown and describedwith references to preferred embodiments thereof, it will be understoodby those skilled in the art that various changes in form and details maybe made therein without departing from the scope of the inventionencompassed by the appended claims. TABLE 1 ANALYSIS REPORT by UniquantSpectrometers configuration: ARL 8410 Rh 60 kV LiF220 LiF420 Ge111 TlAPSample ident = Tailored - 3 Further info = Kappa list = 15-Nov-94Channel list = 23-Sep-99 Calculated as: Elements Spectral impurity data:CAL.209Teflon X-ray path = Vacuum Film type = No supporting film Casenumber = 0 Known Area, % Rest, Diluent/Sample and Mass/Area Eff. Diam. =25.00 mm Eff. Area = 490.6 mm2 KnownConc = 0% Rest = 0% Dil/Sample = 0Viewed Mass = 18000.00 mg Sample Height = 5 mm < means that theconcentration is < 10 ppm <2e means wt % < 2 StdErr. The + in Z + Elmeans involved in Sum = 100% Z wt % StdErr Z wt % StdErr Z wt % StdErrSum Be . . . F 0 0.037 29 + Cu 99.58 0.03 51 Sb < 11 Na < 30 + Zn <2e0.006 52 Te < 12 Mg < 31 + Ga 0.012 0.003 53 I < 13 + Al 0.027 0.012 32Ge <2e 0.003 55 Cs < 14 Si < 33 As < 56 Ba < 15 + P 0.003 0.001 34 Se <Sum La . . . Lu 0.15 0.07 16 + S 0.038 0.003 35 Br < 72 + Hf <2e 0.02216 + So 0.022 0.003 37 Rb < 73 + Ta <2e 0.071 17 + Cl 0.037 0.003 38 Sr< 74 W < 18 + Ar 0.017 0.002 39 Y < 75 Re < 19 + K <2e 0.0008 40 Zr < 76Os < 20 + Ca 0.0050 0.0008 41 Nb < 77 + Ir 0.029 0.008 21 Sc < 42 Mo <78 + Pt 0.017 0.007 22 + Ti 0.015 0.001 44 Ru < 79 Au <2e 0.007 23 V <45 Rh < 80 Hg < 24 Cr < 46 Pd < 81 Tl < 25 + Mn 0.0069 0.0007 47 Ag < 82Pb < 26 + Fe 0.015 0.001 48 + Cd 0.004 0.002 83 Bi < 27 Co < 49 In < 90Th <2e 0.003 28 Ni < 50 Sn < 92 U < Light Elements Noble ElementsLanthanides 4 Be 44 Ru < 57 + La 0.073 0.006 5 B 45 Rh < 58 Ce < 6 C 46Pd < 59 Pr < 7 N 47 Ag < 60 Nd < 8 O 75 Re < 62 + Sm 0.022 0.003 9 E <76 Os < 63 + Eu 0.015 0.002 77 + Ir 0.029 0.008 64 + Gd 0.009 0.002 78 +Pt 0.017 0.007 65 + Tb 0.015 0.002 79 Au <2e 0.007 66 DY < 67 + Ho <2e0.013 68 Er <2e 0.004 69 Tm < 70 Yb <2e 0.005 71 + Lu <2e 0.013KnownConc = 0 REST = 0 D/S = 0

[0406] TABLE 2 ANALYSIS REPORT by Uniquant Spectrometers configuration:ARL 8410 Rh 60 kV LiF220 LiF420 Ge111 TlAP Sample ident = Tailored - 2Further info = Kappa list = 15-Nov-94 Channel list = 23-Sep-99Calculated as: Elements Spectral impurity data: CAL.209Teflon X-ray path= Vacuum Film type = No supporting film Case number = 0 Known Area, %Rest, Diluent/Sample and Mass/Area Eff. Diam. = 25.00 mm Eff. Area =490.6 mm2 KnownConc = 0% Rest = 0% Dil/Sample = 0 Viewed Mass = 18000.00mg Sample Height = 5 mm < means that the concentration is < 10 ppm <2emeans wt % < 2 StdErr. The + in Z + El means involved in Sum = 100% Z wt% StdErr Z wt % StdErr Z wt % StdErr Sum Be . . . F 0 0.036 29 + Cu98.62 0.06 51 Sb < 11 + Na 0.11 0.02 30 + Zn <2e 0.006 52 Te < 12 Mg <31 + Ga 0.007 0.003 53 I < 13 + Al 0.44 0.03 32 Ge <2e 0.003 55 Cs <14 + Si 0.107 0.008 33 As < 56 Ba < 15 + P 0.004 0.001 34 Se < Sum La .. . Lu 0.087 0.072 16 + S 0.19 0.01 35 Br < 72 + Hf < 16 + So 0.12 0.0137 Rb < 73 + Ta <2e 0.071 17 + Cl 0.17 0.01 38 Sr < 74 W < 18 + Ar 0.0270.002 39 Y < 75 Re < 19 + K 0.0065 0.0010 40 Zr < 76 Os < 20 + Ca 0.0130.001 41 Nb < 77 Ir < 21 Sc < 42 Mo < 78 + Pt 0.022 0.008 22 + Ti 0.0150.001 44 Ru < 79 Au <2e 0.007 23 V < 45 Rh < 80 Hg < 24 Cr < 46 Pd < 81Tl < 25 Mn <2e 0.0006 47 Ag < 82 Pb < 26 + Fe 0.044 0.004 48 Cd <2e0.002 83 Bi < 27 Co < 49 In < 90 Th < 28 Ni < 50 Sn < 92 U < LightElements Noble Elements Lanthanides 4 Be 44 Ru < 57 + La 0.059 0.005 5 B45 Rh < 58 Ce <2e 0.003 6 C 46 Pd < 59 Pr <2e 0.003 7 N 47 Ag < 60 Nd<2e 0.002 8 O 75 Re < 62 Sm <2e 0.003 9 F < 76 Os < 63 Eu < 77 Ir < 64Gd < 78 + Pt 0.022 0.008 65 + Tb 0.005 0.002 79 Au <2e 0.007 66 Dy <2e0.008 67 + Ho <2e 0.015 68 Er <2e 0.004 69 Tm < 70 Yb < 71 + Lu <KnownConc = 0 REST = 0 D/S = 0

[0407] TABLE 3 ANALYSIS REPORT by UniQuant Spectrometers configuration:ARL 8410 Rh 60 kV LiF220 LiF420 Ge111 TlAP Sample ident = Tailored - 1Further info = Kappa list = 15-Nov-94 Channel list = 20-Jul-94Calculated as: Elements Spectral impurity data: CAL.209Teflon X-ray path= Vacuum Film type = No supporting film Case number = 0 Known Area, %Rest, Diluent/Sample and Mass/Area Eff. Diam. = 25.00 mm Eff. Area =490.6 mm2 KnownConc = 0% Rest = 0% Dil/Sample = 0 Viewed Mass = 18000.00mg Sample Height = 5 mm < means that the concentration is < 10 ppm <2emeans that Conc < 2 × StdErr Z wt % StdErr Z wt % StdErr Z wt % StdErrSum Be . . . F 0 0.036 29 Cu 99.84 0.03 51 Sb < 11 Na < 30 Zn < 52 Te <12 Mg < 31 Ga 0.007 0.003 53 I < 13 Al < 32 Ge <2e 0.002 55 Cs < 14 Si <33 As < 56 Ba < 15 P < 34 Se < Sum La . . . Lu 0.053 0.071 16 S 0.00890.0008 35 Br < 72 Hf <2e 0.022 16 So < 37 Rb < 73 Ta < 17 Cl 0.017 0.00138 Sr < 74 W < 18 Ar < 39 Y < 75 Re < 19 K <2e 0.0007 40 Zr < 76 Os < 20Ca 0.0024 0.0009 41 Nb < 77 Ir 0.040 0.008 21 Sc <2e 0.001 42 Mo 0.0050.002 78 Pt < 22 Ti 0.003 0.001 44 Ru < 79 Au <2e 0.006 23 V < 45 Rh <80 Hg <2e 0.006 24 Cr < 46 Pd < 81 Tl < 25 Mn < 47 Ag < 82 Pb < 26 Fe <48 Cd < 83 Bi < 27 Co < 49 In < 90 Th 0.009 0.003 28 Ni < 50 Sn < 92 U <Light Elements Noble Elements Lanthanides 4 Be 44 Ru < 57 La 0.030 0.0065 B 45 Rh < 58 Ce < 6 C 46 Pd < 59 Pr < 7 N 47 Ag < 60 Nd < 8 O 75 Re <62 Sm < 9 F < 76 Os < 63 Eu <2e 0.002 77 Ir 0.040 0.008 64 Gd <2e 0.00278 Pt < 65 Tb <2e 0.002 79 Au <2e 0.006 66 Dy < 67 Ho <2e 0.015 68 Er0.014 0.004 69 Tm <2e 0.004 70 Yb < 71 Lu <2e 0.014 KnownConc = 0 REST =0 D/S = 0

[0408] XRF Analyses of Manufactured Ingols Atom No. 14-00-01 Cu 14-00-03Cu 14-00-04 Cu 15-00-001 Cu 14-01-01 Cu 14-01-04 NI 15-01-01 SI ElementAxial Radial Axial Radial Axial Radial Axial Radial Axial Radial AxialRadial Axial Radial Major Elements: 11 Na 0.063 0.11

0.07 0.062

0.048 0.068

0.12 0.004 0.013 12 Mg 13 Al 0.33 0.25 0.103 0.37 0.27 0.63 0.25 0.300.93 0.67 2.11

1.18 1.46 14 Si 0.66 0.56

0.29 0.29 0.6 0.07

0.89 0.51 0.03 0.14 96.56 98.12 19 K 0.0021

0.0023

0.014 23 V 24 Cr 0.002 0.0031 0.0025 25 Mn 26 Fe 0.065 0.012 27 Co 28 Ni

0.0051 0.0053 29 Cu 95.68

98.93 99.29 96.59 89.21 99.38 98.07 98.09 0.012 0.0101 30 Zn 0.00210.002 47 Ag

0.004 50 Sn 72 Hr 0.003 73 Ta 74 W 0.007 0.011 79 Au 82 Po MinorElements 4-9 Be-F 0.11 0.071 0.059 15 P

9.002 0.013 0.018 16 S 0.0042 0.0085

0.012 0.0043 0.0035 0.013 16* So 0.074 0.0057 0.0026 0.0042 0.028 0.1417 Cl 0.026 0.029 0.0

7 8.065 0.021 0.02 0.021 8.034 0.0107 0.0065 9.005 0.004 0.019 18 Ar0.013 0.015 0.013 0.016 0.012 0.016

0.017 0.009 0.006

0.013 0.012 20 Cs 0.0041 0.004

0.0109 0.0025 0.0078

0.0092 0.077 21 Sc

0.0021 0.00

0.00

22 Ti 0.003 0.0037 0.019 0.029 31 Ga 0.008

9.008 0.007 0.006 0.006 0.0038 0.0043 32 Ge 6.001 40 Zr 0.005 0.0270.032 41 No 42 Mo 0.005 44 Ru 45 Rh 0.005 48 Cd 51 Sb 56 Ba 0.006 0.00557-71 0.021 0.011 0.033 0.006 0.023 0.021 0.01 0.017 0.003 0.014 0.690.65 0.004 0.005 Lathanides 75 Rs 77 Ir 0.018 0.031 0.029 0.026 0.0350.038

0.026 90 Th Sum of 100 99.5 82.4 90 99.5 88.1 82.7 94.5 101.7 102.1101.4 100.5 83.4 79.7 Concentr. Before Normal

15-01-04 15-01-03 14-01-07 14-01-08 Atom No. 15-01-02 Fe 14-01-05 Co14-01-06 Au/Ag W/T a/HI V/Cr/Mn/Fe P

/Zn/Sn Sn/Na/K/Mg Element Axial Radial Axial Radial Axial Radial AxialRadial Axial Radial Axial Radial Axial Radial Major Elements: 11 Na

0.025 0.043 0.056

0.065 0.043

1.67 2.02 12 Mg

0.016

13 Al

4.9 3.71

3.36 2.2

0.17 2.00 1.53

14 Si 0.032 0.14 0.073 0.18 0.23 0.74 0.13 0.026 0.018

19 K

23 V

24 Cr 2.71 2.39 25 Mn 0.0091 0.0081 2.05

26 Fe 98.01

0.13 0.13

27 Co 94.6 95.7

28 Ni 0.16 0.18 90.5 90 0.012

29 Cu 0.012 0.814 96.97 97.04 0.025 0.16 0.014 0.24 0.079 0.44 30 Zn0.095 0.032 33.2 25.4

47 Ag

50 Sn 47.9 54.7

72 Hr 0.014 1.78 2 0.018 73 Ta 1.76 1.78 74 W 0.008 1.49 1.5 0.008 0.0330.03

79 Au

82 Po 18.3 18.9 0.087 0.063 Minor Elements 4-9 Be-F 15 P 0.0023

0.004 0.0037 0.0025 0.0031 0.0097

16 S 0.0532 0.0066 0.0069 0.0053 16* So 0.0$ 0.012 0.0092

0.038

17 Cl 0.004 0.0044 0.0047 0.0034 0.02 0.025 0.0044 0.0059 0.011 0.0520.031 0.053 0.005 0.013 18 Ar 0.012 0.913 0.011 0.01 0.014

0.018 0.019 0.009 0.01 20 Cs 0.0

0.0075 0.0087

0.0025 0.0

0.0

21 Sc 0.025 0.0026 0.0022 0.0033 0.0036 0.002 0.007 22 Ti 0.003 31 Ga0.002 32 Ge 40 Zr

0.012 0.019 0.017 0.00

0.0

0.097 0.016 0.02

0.043 41 No 42 Mo 44 Ru 0.011 45 Rh 48 Cd 0.003 0.025 0.014 0.041 0.02951 Sb 0.015 0.023 56 Ba 0.006 57-71 0.02 0.02 0.012 0.003 0.58 0.570.031 0.035 0.021 0.025 Lathanides 75 Rs 0.021 77 Ir 0.025 0.038 90 Th0.008 0.085 0.006 Sum of 96.3 97.8 102 101.3 100.1 100.1 101 101.9 100.129.9 111.4 116.8

Concentr. Before Normal

[0409] TABLE 5 Quantum Catalytics, LLC ANALYSIS REPORT by UniquantOLD.347 of 19-Jun-01 Today 19-Jun-01 Spectrometers configuration: ARL8410 Rh 60 kV LiF220 LiF420 Ge111 TlAP Sample ident = 14-01-01 AXIALFurther info = 14-01-01 AXIAL 6/19 Kappa list = 15-Nov-94 Channel list =18-Jun-01 Calculated as: Elements Spectral impurity data: CAL.909 Teflon(7/94) X-ray path = Vacuum Film type = No supporting film Case number =0 Known Area, % Rest, Diluent/Sample and Mass/Area Eff. Diam. = 25.00 mmEff. Area = 490.6 mm2 KnownConc = 0% Rest = 0% Dil/Sample = 0 ViewedMass = 18000.00 mg Sample Height = 5 mm < means that the concentrationis < 20 ppm <2e means wt % < 2 StdErr. The + in Z + E1 means involved inSum = 100% Z wt % StdErr Z wt % StdErr Z wt % StdErr Sum Be . . . F 00.034 29 + Cu 98.07 0.07 51 Sb < 11 + Na 0.046 0.009 30 + Zn < 52 Te <12 Mg < 31 + Ga 0.006 0.003 53 I < 13 + Al 0.93 0.04 32 Ge < 55 Cs <14 + Si 0.89 0.04 33 As < 56 Ba <2e 0.003 15 + P < 34 Se < Sum La . . .Lu 0.003 0.058 16 S 35 Br < 72 + Hf < 16 + So 0.0087 0.0008 37 Rb < 73 +Ta < 17 + Cl 0.0107 0.0010 38 Sr < 74 W < 18 + Ar 0.009 0.002 39 Y < 75Re < 19 K < 40 Zr < 76 Os < 20 + Ca 0.0078 0.0008 41 Nb < 77 + Ir 0.0250.008 21 Sc < 42 Mo < 78 Pt <2e 0.007 22 Ti < 44 Ru < 79 Au < 23 V < 45Rh <2e 0.002 80 Hg <2e 0.006 24 Cr < 46 Pd < 81 Tl < 25 Mn < 47 Ag <2e0.002 82 Pb <2e 0.003 26 Fe < 48 Cd < 83 Bi < 27 Co < 49 In < 90 Th <2e0.003 28 Ni < 50 Sn < 92 U < Light Elements Noble Elements Lanthanides 4Be 44 Ru < 57 La < 5 B 45 Rh <2e 0.002 58 Ce < 6 C 46 Pd < 59 Pr < 7 N47 Ag <2e 0.002 60 Nd < 8 O 75 Re < 62 Sm < 9 F < 76 Os < 63 Eu <2e0.001 77 + Ir 0.025 0.008 64 Gd < 78 Pt <2e 0.007 65 Tb < 79 Au < 66 Dy< 67 Ho < 68 Br < 69 Tm < 70 Yb < 71 + Lu < KnownConc = 0 REST = 0 D/S =0

[0410] TABLE 6 Quantum Catalytics, LLC ANALYSIS REPORT by UniquantOLD.346 of 19-Jun-01 Today 19-Jun-01 Spectrometers configuration: ARL8410 Rh 60 kv LiF220 LiF420 Ge111 TlAP Sample ident = 14-01-01 RADIALFurther info = 14-01-01 RADIAL 6/19 Kappa list = 15-Nov-94 Channel list= 18-Jun-01 Calculated as: Elements Spectral impurity data: CAL.909Teflon (7/94) X-ray path = Vacuum Film type = No supporting film Casenumber = 0 Known Area, % Rest, Diluent/Sample and Mass/Area Eff. Diam. =25.00 mm Eff. Area = 490.6 mm2 KnownConc = 0% Rest = 0% Dil/Sample = 0Viewed Mass = 18000.00 mg Sample Height = 5 mm < means that theconcentration is < 20 ppm <2e means wt % < 2 StdErr. The + in Z + Elmeans involved in Sum = 100% Z wt % StdErr Z wt % StdErr Z wt % StdErrSum Be . . . F 0.071 0.036 29 + Cu 98.69 0.06 51 Sb < 11 + Na 0.0680.009 30 + Zn < 52 Te < 12 Mg < 31 + Ga 0.006 0.003 53 I < 13 + Al 0.670.03 32 Ge < 55 Cs < 14 + Si 0.51 0.03 33 As < 56 Ba < 15 + P < 34 Se <Sum La . . . Lu 0.014 0.062 16 S 35 Br < 72 + Hf < 16 + So 0.0026 0.000437 Rb < 73 + Ta < 17 + Cl 0.0065 0.0009 38 Sr < 74 W < 18 + Ar 0.0060.001 39 Y < 75 Re < 19 K < 40 Zr < 76 Os < 20 Ca < 41 Nb < 77 + Ir <2e0.008 21 + Sc 0.0040 0.0007 42 + Mo 0.005 0.002 78 Pt < 22 Ti < 44 Ru<2e 0.002 79 Au <2e 0.007 23 V < 45 Rh < 80 Hg < 24 + Cr < 46 Pd < 81 Tl< 25 Mn < 47 + Ag 0.004 0.002 82 Pb < 26 Fe < 48 Cd < 83 Bi < 27 + Co <49 In < 90 Th <2e 0.003 28 Ni < 50 Sn < 92 U < Light Elements NobleElements Lanthanides 4 Be 44 Ru <2e 0.002 57 La < 5 B 45 Rh < 58 Ce < 6C 46 Pd < 59 Pr < 7 N 47 + Ag 0.004 0.002 60 Nd < 8 O 75 Re < 62 Sm < 9F <2e 0.036 76 Os < 63 Eu < 77 + Ir <2e 0.008 64 Gd < 78 Pt < 65 Tb < 79Au <2e 0.007 66 Dy < 67 Ho < 68 + Er 0.012 0.003 69 Tm < 70 Yb < 71 + Lu< KnownConc = 0 REST = 0 D/S = 0

[0411] TABLE 7 Quantum Catalytics, LLC ANALYSIS REPORT by UniquantOLD.236 of 23-Apr-01 Today 23-Apr-01 Spectrometers configuration: ARL8410 Rh 60 kV LiF220 LiF420 Ge111 TlAP Sample ident = 14-01-01 CuSECTION TOP Further info = 14-01-01 MIDDLE SECTION TOP FACE AXIAL Kappalist = 15-Nov-94 Channel list = 19-Apr-01 Calculated as: ElementsSpectral impurity data: CAL.909 Teflon (7/94) X-ray path = Vacuum Filmtype = No supporting film Case number = 0 Known Area, % Rest,Diluent/Sample and Mass/Area Eff. Diam. = 25.00 mm Eff. Area = 490.6 mm2KnownConc = 0% Rest = 0% Dil/Sample = 0 Viewed Mass = 18000.00 mg SampleHeight = 5 mm < means that the concentration is < 20 ppm <2e means wt %< 2 StdErr. The + in Z + El means involved in Sum = 100% Z wt % StdErr Zwt % StdErr Z wt % StdErr Sum Be . . . F 0 0.037 29 + Cu 99.71 0.03 51Sb < 11 + Na 0.098 0.011 30 + Zn < 52 Te < 12 Mg <2e 0.004 31 Ga <2e0.003 53 I < 13 + Al 0.066 0.005 32 Ge < 55 + Cs 0.007 0.003 14 Si < 33As < 56 Ba < 15 + P < 34 Se < Sum La . . . Lu 0.024 0.074 16 + S 0.0140.001 35 Br < 72 + Hf < 16 So 37 Rb < 73 + Ta < 17 + Cl 0.028 0.002 38Sr < 74 W < 18 + Ar 0.019 0.002 39 Y < 75 Re < 19 + K 0.0021 0.0007 40Zr < 76 Os < 20 + Ca < 41 Nb < 77 + Ir 0.024 0.008 21 Sc < 42 Mo < 78 Pt< 22 + Ti 0.0021 0.0009 44 Ru < 79 Au < 23 V < 45 Rh < 80 Hg < 24 Cr <46 Pd < 81 Tl < 25 Mn < 47 Ag < 82 Pb < 26 Fe < 48 + Cd 0.004 0.002 83Bi < 27 Co < 49 In < 90 + Th 0.007 0.003 28 Ni < 50 Sn < 92 U < LightElements Noble Elements Lanthanides 4 Be 44 Ru < 57 + La 0.015 0.004 5 B45 Rh < 58 Ce < 6 C 46 Pd < 59 Pr < 7 N 47 Ag < 60 Nd < 8 O 75 Re < 62Sm < 9 F < 76 Os < 63 Eu < 77 + Ir 0.024 0.008 64 Gd <2e 0.002 78 Pt <65 Tb < 79 Au < 66 Dy < 67 Ho < 68 Er <2e 0.004 69 Tm <2e 0.005 70 Yb <71 + Lu < KnownConc = 0 REST = 0 D/S = 0

[0412] TABLE 8 Quantum Catalytics, LLC ANALYSIS REPORT by UniquantOLD.244 of 19-Apr-01 Today 24-Apr-01 Spectrometers configuration: ARL8410 Rh 60 kV LiF220 LiF420 Ge111 TlAP Sample ident = 14-01-01 MIDBOTTOM FACE Further info = 14-01-01 MIDDLE SECTION BOTTOM FCE AXIALKappa list = 15-Nov-94 Channel list = 19-Apr-01 Calculated as: ElementsSpectral impurity data: CAL.909 Teflon (7/94) X-ray path = Vacuum Filmtype = No supporting film Case number = 0 Known Area, % Rest,Diluent/Sample and Mass/Area Eff. Diam. = 25.00 mm Eff. Area = 490.6 mm2KnownConc = 0% Rest = 0% Dil/Sample = 0 Viewed Mass = 18000.00 mg SampleHeight = 5 mm < means that the concentration is < 20 ppm <2e means wt %< 2 StdErr. The + in Z + El means involved in Sum = 100% Z wt % StdErr Zwt % StdErr Z wt % StdErr Sum Be . . . F 0 0.037 29 + Cu 98.42 0.06 51Sb < 11 + Na 0.21 0.01 30 + Zn < 52 Te < 12 + Mg 0.013 0.004 31 + Ga0.006 0.003 53 I < 13 + Al 0.80 0.04 32 Ge < 55 Cs < 14 + Si 0.34 0.0233 As < 56 Ba <2e 0.003 15 + P < 34 Se < Sum La . . . Lu 0.018 0.07116 + S 0.031 0.003 35 Br < 72 + Hf <2e 0.022 16 So 37 Rb < 73 + Ta <17 + Cl 0.070 0.006 38 + Sr 0.0024 0.0010 74 W < 18 + Ar 0.019 0.002 39Y < 75 Re < 19 + K 0.020 0.002 40 Zr < 76 Os <2e 0.006 20 + Ca 0.0120.001 41 Nb < 77 + Ir 0.033 0.008 21 Sc < 42 + Mo <2e 0.002 78 Pt < 22 +Ti 0.003 0.001 44 Ru < 79 Au <2e 0.006 23 V < 45 Rh <2e 0.002 80 Hg <2e0.006 24 Cr < 46 Pd < 81 Tl < 25 Mn < 47 Ag < 82 + Pb 0.009 0.003 26 Fe<2e 0.001 48 + Cd 0.004 0.002 83 Bi < 27 + Co < 49 In < 90 Th < 28 Ni <50 Sn < 92 U < Light Elements Noble Elements Lanthanides 4 Be 44 Ru < 57La <2e 0.005 5 B 45 Rh <2e 0.002 58 Ce < 6 C 46 Pd < 59 Pr < 7 N 47 Ag <60 Nd < 8 O 75 Re < 62 Sm < 9 F < 76 Os <2e 0.006 63 Eu <2e 0.002 77 +Ir 0.033 0.008 64 Gd < 78 Pt < 65 Tb < 79 Au <2e 0.006 66 Dy < 67 Ho <68 + Er 0.013 0.004 69 Tm < 70 Yb < 71 + Lu < KnownConc = 0 REST = 0 D/S= 0

[0413] TABLE 9 Quantum Catalytics, LLC ANALYSIS REPORT by UniquantOLD.252 of 19-Apr-01 Today 25-Apr-01 Spectrometers configuration: ARL8410 Rh 60 kV LiF220 LiF420 Ge111 TlAP Sample ident = 14-01-01 MID SECTTOP FAC Further info = 14-01-01 MIDDLE SECTION TOP FACE 4/25/01 Kappalist = 15-Nov-94 Channel list = 19-Apr-01 Calculated as: ElementsSpectral impurity data: CAL.909 Teflon (7/94) X-ray path = Vacuum Filmtype = No supporting film Case number = 0 Known Area, % Rest,Diluent/Sample and Mass/Area Eff. Diam. = 25.00 mm Eff. Area = 490.6 mm2KnownConc = 0% Rest = 0% Dil/Sample = 0 Viewed Mass = 18000.00 mg SampleHeight = 5 mm < means that the concentration is < 20 ppm <2e means wt %< 2 StdErr. The + in Z + El means involved in Sum = 100% Z wt % StdErr Zwt % StdErr Z wt % StdErr Sum Be . . . F 0 0.038 29 + Cu 99.66 0.03 51Sb < 11 + Na 0.034 0.011 30 + Zn < 52 Te < 12 Mg < 31 Ga <2e 0.003 53 I< 13 + Al 0.15 0.01 32 Ge < 55 Cs < 14 + Si 0.033 0.005 33 As <2e 0.00456 Ba <2e 0.003 15 + P < 34 Se < Sum La . . . Lu 0.026 0.075 16 + S0.017 0.002 35 Br < 72 + Hf < 16 So 37 Rb < 73 + Ta < 17 + Cl 0.0270.002 38 + Sr 0.003 0.001 74 W < 18 + Ar 0.017 0.002 39 Y < 75 Re < 19 +K 0.0021 0.0007 40 Zr < 76 Os <2e 0.007 20 + Ca 0.0056 0.0007 41 Nb <77 + Ir 0.026 0.008 21 Sc < 42 Mo < 78 Pt < 22 + Ti 0.0023 0.0010 44 Ru< 79 Au < 23 V < 45 Rh < 80 Hg < 24 Cr < 46 Pd < 81 Tl < 25 Mn < 47 Ag <82 Pb < 26 Fe < 48 Cd < 83 Bi <2e 0.005 27 Co < 49 In < 90 Th <2e 0.00328 Ni < 50 Sn < 92 U < Light Elements Noble Elements Lanthanides 4 Be 44Ru < 57 + La 0.021 0.004 5 B 45 Rh < 58 Ce < 6 C 46 Pd < 59 Pr < 7 N 47Ag < 60 Nd < 8 O 75 Re < 62 Sm < 9 F < 76 Os <2e 0.007 63 Eu < 77 + Ir0.026 0.008 64 Gd < 78 Pt < 65 Tb < 79 Au < 66 Dy < 67 Ho < 68 Er < 69Tm <2e 0.005 70 Yb < 71 + Lu < KnownConc = 0 REST = 0 D/S = 0

[0414] TABLE 10 Quantum Catalytics, LLC ANALYSIS REPORT by UniquantOLD.255 of 19-Apr-01 Today 25-Apr-01 Spectrometers configuration: ARL8410 Rh 60 kV LiF220 LiF420 Ge111 TlAP Sample ident = 14-01-01 MID SECTTOP FAC Further info = 14-01-01 MIDDLE SECTION TOP FACE 4/25/01 Kappalist = 15-Nov-94 Channel list = 19-Apr-01 Calculated as: ElementsSpectral impurity data: CAL.909 Teflon (7/94) X-ray path = Vacuum Filmtype = No supporting film Case number = 0 Known Area, % Rest,Diluent/Sample and Mass/Area Eff. Diam. = 25.00 mm Eff. Area = 490.6 mm2KnownConc = 0% Rest = 0% Dil/Sample = 0 Viewed Mass = 18000.00 mg SampleHeight = 5 mm < means that the concentration is < 20 ppm <2e means wt %< 2 StdErr. The + in Z + El means involved in Sum = 100% Z wt % StdErr Zwt % StdErr Z wt % StdErr Sum Be . . . F 0 0.035 29 + Cu 99.70 0.03 51Sb < 11 + Na <2e 0.011 30 + Zn < 52 Te < 12 Mg < 31 Ga <2e 0.003 53 I <13 + Al 0.14 0.01 32 Ge < 55 Cs < 14 + Si 0.028 0.006 33 As < 56 Ba <15 + P < 34 Se < Sum La . . . Lu 0.019 0.075 16 + S 0.018 0.002 35 Br <72 + Hf < 16 So 37 Rb < 73 + Ta < 17 + Cl 0.028 0.002 38 Sr < 74 W <18 + Ar 0.020 0.002 39 Y < 75 Re < 19 + K 0.0033 0.0007 40 Zr < 76 Os <20 + Ca 0.0058 0.0007 41 Nb < 77 + Ir 0.021 0.008 21 Sc < 42 Mo < 78 Pt<2e 0.008 22 + Ti 0.0028 0.0009 44 Ru < 79 Au < 23 V < 45 Rh < 80 Hg <2e0.006 24 Cr < 46 Pd < 81 Tl < 25 Mn < 47 Ag <2e 0.002 82 Pb < 26 Fe < 48Cd < 83 Bi < 27 Co < 49 In < 90 Th 0.006 0.003 28 Ni < 50 Sn < 92 U <Light Elements Noble Elements Lanthanides 4 Be 44 Ru < 57 + La 0.0160.003 5 B 45 Rh < 58 Ce < 6 C 46 Pd < 59 Pr < 7 N 47 Ag <2e 0.002 60 Nd< 8 O 75 Re < 62 Sm < 9 F < 76 Os < 63 Eu < 77 + Ir 0.021 0.008 64 Gd <78 Pt <2e 0.008 65 Tb < 79 Au < 66 Dy < 67 Ho < 68 Er < 69 Tm <2e 0.00570 Yb < 71 + Lu < KnownConc = 0 REST = 0 D/S = 0

[0415] TABLE 11 Quantum Catalytics, LLC ANALYSIS REPORT by UniquantOLD.259 of 19-Apr-01 Today 26-Apr-01 Spectrometers configuration: ARL8410 Rh 60 kV LiF220 LiF420 Ge111 TlAP Sample ident = 14-01-01 BOTBOTTOM Further info = 14-01-01 MIDDLE SECTION BOT FACE 4/25/01 Kappalist = 15-Nov-94 Channel list = 19-Apr-01 Calculated as: ElementsSpectral impurity data : CAL.909 Teflon (7/94) X-ray path = Vacuum Filmtype = No supporting film Case number = 0 Known Area, % Rest,Diluent/Sample and Mass/Area Eff. Diam. = 25.00 mm Eff. Area = 490.6 mm2KnownConc = 0% Rest = 0% Dil/Sample = 0 Viewed Mass = 18000.00 mg SampleHeight = 5 mm < means that the concentration is < 20 ppm <2e means wt %< 2 StdErr. The + in Z + El means involved in Sum = 100% Z wt % StdErr Zwt % StdErr Z wt % StdErr Sum Be . . . F 0 0.037 29 + Cu 98.53 0.06 51Sb < 11 + Na 0.14 0.01 30 + Zn < 52 Te < 12 Mg <2e 0.004 31 Ga <2e 0.00353 I < 13 + Al 0.78 0.04 32 Ge < 55 Cs < 14 + Si 0.35 0.02 33 As < 56 Ba< 15 + P < 34 Se < Sum La . . . Lu 0.024 0.071 16 S 35 Br < 72 + Hf <16 + So 0.032 0.003 37 Rb < 73 + Ta < 17 + Cl 0.061 0.005 38 Sr < 74 W <18 + Ar 0.018 0.002 39 Y < 75 Re < 19 + K 0.021 0.002 40 Zr < 76 Os <20 + Ca 0.013 0.001 41 Nb < 77 + Ir 0.026 0.008 21 Sc < 42 Mo < 78 Pt <22 Ti <2e 0.001 44 Ru < 79 Au < 23 V < 45 Rh < 80 Hg <2e 0.006 24 Cr <46 Pd < 81 Tl < 25 + Mn < 47 Ag < 82 + Pb 0.007 0.003 26 + Fe 0.0030.001 48 Cd < 83 Bi < 27 Co < 49 In < 90 Th <2e 0.003 28 Ni < 50 Sn < 92U < Light Elements Noble Elements Lanthanides 4 Be 44 Ru < 57 La <2e0.004 5 B 45 Rh < 58 Ce < 6 C 46 Pd < 59 Pr < 7 N 47 Ag < 60 Nd < 8 O 75Re < 62 Sm < 9 F < 76 Os < 63 + Eu 0.005 0.002 77 + Ir 0.026 0.008 64 Gd<2e 0.002 78 Pt < 65 Tb < 79 Au < 66 Dy < 67 Ho < 68 + Er 0.012 0.004 69Tm < 70 Yb < 71 + Lu < KnownConc = 0 REST = 0 D/S = 0

[0416] TABLE 12 Quantum Catalytics, LLC ANALYSIS REPORT by UniquantOLD.260 of 19-Apr-01 Today 26-Apr-01 Spectrometers configuration: ARL8410 Rh 60 kV LiF220 LiF420 Ge111 TlAP Sample ident = 14-01-01 BOTBOTTOM Further info = 14-01-01 MID SECT BOT FACE 4/25/01 BTB Kappa list= 15-Nov-94 Channel list = 19-Apr-01 Calculated as: Elements Spectralimpurity data : CAL.909 Teflon (7/94) X-ray path = Vacuum Film type = Nosupporting film Case number = 0 Known Area, % Rest, Diluent/Sample andMass/Area Eff. Diam. = 25.00 mm Eff. Area = 490.6 mm2 KnownConc = 0%Rest = 0% Dil/Sample = 0 Viewed Mass = 18000.00 mg Sample Height = 5 mm< means that the concentration is < 20 ppm <2e means wt % < 2 StdErr.The + in Z + El means involved in Sum = 100% Z wt % StdErr Z wt % StdErrZ wt % StdErr Sum Be . . . F 0 0.036 29 + Cu 98.55 0.06 51 Sb < 11 + Na0.12 0.01 30 + Zn < 52 Te < 12 Mg <2e 0.004 31 + Ga 0.010 0.003 53 I <13 + Al 0.77 0.04 32 Ge <2e 0.002 55 + Cs 0.006 0.003 14 + Si 0.34 0.0233 As <2e 0.004 56 Ba 0.006 0.003 15 + P < 34 Se < Sum La . . . Lu 0.0130.071 16 + S 0.034 0.003 35 Br < 72 + Hf <2e 0.022 16 So 37 Rb < 73 + Ta< 17 + Cl 0.064 0.005 38 Sr < 74 W < 18 + Ar 0.018 0.002 39 Y < 75 Re <19 + K 0.021 0.002 40 Zr < 76 Os <2e 0.007 20 + Ca 0.014 0.001 41 Nb <77 + Ir 0.018 0.007 21 Sc < 42 Mo <2e 0.002 78 Pt < 22 Ti < 44 Ru < 79 +Au 0.014 0.007 23 V < 45 Rh < 80 Hg <2e 0.006 24 Cr < 46 Pd < 81 Tl < 25Mn < 47 Ag <2e 0.002 82 Pb <2e 0.003 26 Fe <2e 0.001 48 Cd < 83 + Bi0.013 0.005 27 Co < 49 In < 90 Th <2e 0.003 28 Ni < 50 Sn < 92 U < LightElements Noble Elements Lanthanides 4 Be 44 Ru < 57 + La <2e 0.005 5 B45 Rh < 58 Ce <2e 0.002 6 C 46 Pd < 59 Pr < 7 N 47 Ag <2e 0.002 60 Nd <8 O 75 Re < 62 Sm < 9 F < 76 Os <2e 0.007 63 Eu < 77 + Ir 0.018 0.007 64Gd < 78 Pt < 65 Tb <2e 0.002 79 + Au 0.014 0.007 66 Dy < 67 Ho < 68 Er <69 Tm < 70 Yb < 71 + Lu < KnownConc = 0 REST = 0 D/S = 0

[0417] TABLE 13 Quantum Catalytics, LLC ANALYSIS REPORT by UniquantOLD.261 of 19-Apr-01 Today 26-Apr-01 Spectrometers configuration: ARL8410 Rh 60 kV LiF220 LiF420 Ge111 TlAP Sample ident = 14-01-01 BOTBOTTOM Further info = 14-01-01 MID SECT BOT FACE 4/25/01 3 HR Kappa list= 15-Nov-94 Channel list = 19-Apr-01 Calculated as: Elements Spectralimpurity data : CAL.909 Teflon (7/94) X-ray path = Vacuum Film type = Nosupporting film Case number = 0 Known Area, % Rest, Diluent/Sample andMass/Area Eff. Diam. = 25.00 mm Eff. Area = 490.6 mm2 KnownConc = 0%Rest = 0% Dil/Sample = 0 Viewed Mass = 18000.00 mg Sample Height = 5 mm< means that the concentration is < 20 ppm <2e means wt % < 2 StdErr.The + in Z + El means involved in Sum = 100% Z wt % StdErr Z wt % StdErrZ wt % StdErr Sum Be . . . F 0 0.038 29 + Cu 98.50 0.06 51 Sb < 11 + Na0.15 0.01 30 + Zn < 52 Te < 12 + Mg 0.014 0.004 31 + Ga 0.009 0.003 53 I< 13 + Al 0.79 0.04 32 Ge < 55 Cs < 14 + Si 0.35 0.02 33 As < 56 Ba <15 + P < 34 Se < Sum La . . . Lu 0.016 0.071 16 + S 0.036 0.003 35 Br <72 + Hf < 16 So 37 Rb < 73 + Ta < 17 + Cl 0.062 0.005 38 Sr < 74 W <18 + Ar 0.018 0.002 39 Y < 75 Re < 19 + K 0.020 0.002 40 Zr < 76 Os <20 + Ca 0.0108 0.0010 41 Nb < 77 + Ir 0.016 0.007 21 + Sc 0.0020 0.000942 Mo < 78 Pt <2e 0.007 22 + Ti <2e 0.001 44 Ru < 79 Au < 23 V < 45 Rh <80 Hg <2e 0.006 24 Cr < 46 Pd < 81 Tl < 25 Mn < 47 Ag <2e 0.002 82 Pb0.006 0.003 26 Fe <2e 0.001 48 + Cd 0.004 0.002 83 Bi < 27 + Co < 49 In< 90 Th <2e 0.003 28 Ni < 50 Sn < 92 U < Light Elements Noble ElementsLanthanides 4 Be 44 Ru < 57 La <2e 0.004 5 B 45 Rh < 58 Ce < 6 C 46 Pd <59 Pr < 7 N 47 Ag <2e 0.002 60 Nd < 8 O 75 Re < 62 Sm < 9 F < 76 Os < 63Eu < 77 + Ir 0.016 0.007 64 Gd < 78 Pt <2e 0.007 65 Tb < 79 Au < 66 Dy <67 Ho < 68 + Er 0.013 0.004 69 Tm < 70 Yb < 71 + Lu < KnownConc = 0 REST= 0 D/S = 0

[0418] TABLE 14 Quantum Catalytics, LLC ANALYSIS REPORT by UniquantOLD.320 of 24-May-01 Today 25-May-01 Spectrometers configuration: ARL8410 Rh 60 kV LiF220 LiF420 Ge111 TlAP Sample ident = 14-01-04 Ni AXIALBLK Further info = 14-01-04 Ni AXIAL BLK 5/25 Kappa list = 15-Nov-94Channel list = 24-May-01 Calculated as: Elements Spectral impurity data: CAL.909 Teflon (7/94) X-ray path = Vacuum Film type = No supportingfilm Case number = 0 Known Area, % Rest, Diluent/Sample and Mass/AreaEff. Diam. = 25.00 mm Eff. Area = 490.6 mm2 KnownConc = 0% Rest = 0%Dil/Sample = 0 Viewed Mass = 18000.00 mg Sample Height = 5 mm < meansthat the concentration is < 20 ppm <2e means wt % < 2 StdErr. The + inZ + El means involved in Sum = 100% Z wt % StdErr Z wt % StdErr Z wt %StdErr Sum Be . . . F 0 0.035 29 Cu < 51 Sb < 11 + Na 0.031 0.009 30 Zn< 52 Te < 12 Mg < 31 Ga < 53 I < 13 + Al 2.11 0.07 32 Ge < 55 Cs < 14 +Si 0.030 0.005 33 As < 56 Ba <2e 0.003 15 + P 0.0020 0.0003 34 Se < SumLa . . . Lu 0.69 1.22 16 S 35 Br < 72 Hf <2e 0.007 16 + So 0.0042 0.000437 Rb < 73 + Ta < 17 + Cl < 38 Sr < 74 + W < 18 Ar < 39 Y < 75 Re < 19 K< 40 + Zr 0.027 0.002 76 Os < 20 Ca < 41 Nb < 77 Ir < 21 + Sc 0.00240.0008 42 Mo <2e 0.002 78 Pt < 22 Ti < 44 Ru <2e 0.002 79 Au < 23 V <45 + Rh 0.005 0.002 80 Hg < 24 Cr < 46 Pd < 81 Tl < 25 Mn < 47 Ag < 82Pb < 26 Fe < 48 Cd < 83 Bi < 27 Co < 49 In < 90 Th < 28 + Ni 97.10 0.0850 Sn < 92 U < Light Elements Noble Elements Lanthanides 4 Be 44 Ru <2e0.002 57 La < 5 B 45 + Rh 0.005 0.002 58 Ce < 6 C 46 Pd < 59 Pr < 7 N 47Ag < 60 Nd < 8 O 75 Re < 62 Sm < 9 F < 76 Os < 63 Eu < 77 Ir < 64 Gd <78 Pt < 65 Tb < 79 Au < 66 + Dy < 67 + Ho < 68 Er < 69 Tm < 70 + Yb 0.690.27 71 Lu < KnownConc = 0 REST = 0 D/S = 0

[0419] TABLE 15 Quantum Catalytics, LLC ANALYSIS REPORT by UniquantOLD.321 of 24-May-01 Today 25-May-01 Spectrometers configuration: ARL8410 Rh 60 kV LiF220 LiF420 Ge111 TlAP Sample ident = 14-01-04 Ni RADIALBLK Further info = 14-01-04 Ni RADIAL BLK 5/25 Kappa list = 15-Nov-94Channel list = 24-May-01 Calculated as: Elements Spectral impurity data: CAL.909 Teflon (7/94) X-ray path = Vacuum Film type = No supportingfilm Case number = 0 Known Area, % Rest, Diluent/Sample and Mass/AreaEff. Diam. = 25.00 mm Eff. Area = 490.6 mm2 KnownConc = 0% Rest = 0%Dil/Sample = 0 Viewed Mass = 18000.00 mg Sample Height = 5 mm < meansthat the concentration is < 20 ppm <2e means wt % < 2 StdErr. The + inZ + El means involved in Sum = 100% Z wt % StdErr Z wt % StdErr Z wt %StdErr Sum Be . . . F 0 0.037 29 Cu < 51 Sb < 11 + Na 0.12 0.01 30 Zn <52 Te < 12 Mg < 31 Ga < 53 I < 13 + Al 2.57 0.07 32 + Ge 0.005 0.002 55Cs <2e 0.002 14 + Si 0.14 0.01 33 As < 56 Ba 0.006 0.003 15 + P < 34 Se< Sum La . . . Lu 0.65 1.21 16 S 35 Br < 72 Hf <2e 0.007 16 + So 0.0260.002 37 Rb < 73 + Ta < 17 + Cl 0.0050 0.0007 38 Sr < 74 + W < 18 + Ar0.010 0.001 39 Y < 75 Re <2e 0.006 19 + K 0.0048 0.0007 40 + Zr 0.0320.003 76 Os < 20 + Ca 0.011 0.001 41 Nb < 77 Ir <2e 0.006 21 Sc < 42 Mo<2e 0.002 78 Pt < 22 Ti < 44 Ru < 79 Au < 23 V < 45 Rh < 80 Hg <2e 0.00424 Cr < 46 Pd < 81 Tl < 25 Mn < 47 Ag <2e 0.002 82 Pb < 26 Fe < 48 Cd<2e 0.002 83 Bi < 27 Co < 49 In < 90 Th <2e 0.002 28 + Ni 96.43 0.09 50Sn < 92 U <2e 0.002 Light Elements Noble Elements Lanthanides 4 Be 44 Ru< 57 La < 5 B 45 Rh < 58 Ce < 6 C 46 Pd < 59 Pr < 7 N 47 Ag <2e 0.002 60Nd < 8 O 75 Re <2e 0.006 62 Sm < 9 F < 76 Os < 63 Eu < 77 Ir <2e 0.00664 Gd < 78 Pt < 65 Tb <2e 0.003 79 Au < 66 + Dy < 67 + Ho < 68 Er < 69Tm < 70 + Yb 0.64 0.27 71 Lu < KnownConc = 0 REST = 0 D/S = 0

[0420] TABLE 16 Quantum Catalytics, LLC ANALYSIS REPORT by UniquantOLD.327 of 1-Jun-01 Today 4-Jun-01 Spectrometers configuration: ARL 8410Rh 60 kV LiF220 LiF420 Ge111 TlAP Sample ident = 14-01-05 Co AXIAL TOPFurther info = 14-01-05 CO AXIAL TOP Kappa list = 15-Nov-94 Channel list= 24-May-01 Calculated as: Elements Spectral impurity data: CAL.909Teflon (7/94) X-ray path = Vacuum Film type = No supporting film Casenumber = 0 Known Area, % Rest, Diluent/Sample and Mass/Area Eff. Diam. =25.00 mm Eff. Area = 490.6 mm2 KnownConc = 0% Rest = 0% Dil/Sample = 0Viewed Mass = 18000.00 mg Sample Height = 5 mm < means that theconcentration is < 20 ppm <2e means wt % < 2 StdErr. The + in Z + Elmeans involved in Sum = 100% Z wt % StdErr Z wt % StdErr Z wt % StdErrSum Be . . . F 0 0.88 29 Cu < 51 Sb < 11 + Na 0.026 0.008 30 Zn < 52 Te< 12 Mg < 31 Ga <2e 0.002 53 I < 13 + Al 4.9 0.1 32 Ge < 55 Cs < 14 + Si0.073 0.006 33 As < 56 + Ba 0.006 0.003 15 + P 0.0040 0.0004 34 Se < SumLa . . . Lu 0.02 10.08 16 S 35 Br < 72 + Hf 0.014 0.006 16 + So < 37 Rb< 73 Ta < 17 + Cl 0.0047 0.0006 38 Sr < 74 W < 18 + Ar 0.011 0.001 39 Y< 75 Re < 19 K < 40 + Zr 0.019 0.002 76 Os < 20 + Ca 0.0075 0.0007 41 Nb< 77 Ir <2e 0.005 21 + Sc 0.0022 0.0006 42 Mo < 78 Pt < 22 Ti < 44 Ru <79 Au < 23 V < 45 Rh < 80 Hg <2e 0.004 24 Cr < 46 Pd < 81 Tl < 25 + Mn0.0091 0.0008 47 Ag < 82 Pb <2e 0.002 26 + Fe 0.13 0.01 48 Cd 0.0030.002 83 Bi < 27 + Co 94.6 0.1 49 In < 90 Th <2e 0.002 28 + Ni 0.16 0.0150 Sn < 92 U < Light Elements Noble Elements Lanthanides 4 Be 44 Ru < 57La < 5 B 45 Rh < 58 Ce < 6 C 46 Pd < 59 Pr < 7 N 47 Ag < 60 Nd < 8 O 75Re < 62 Sm < 9 + F < 76 Os < 63 Eu <2e 0.002 77 Ir <2e 0.005 64 + Gd0.016 0.003 78 Pt < 65 Tb < 79 Au < 66 Dy < 67 + Ho < 68 + Er < 69 Tm <70 + Yb < 71 + Lu < KnownConc = 0 REST = 0 D/S = 0

[0421] TABLE 17 Quantum Catalytics, LLC ANALYSIS REPORT by UniquantOLD.328 of 1-Jun-01 Today 4-Jun-01 Spectrometers configuration: ARL 8410Rh 60 kV LiF220 LiF420 Ge111 TlAP Sample ident = 14-01-05 Co RADIALFurther info = 14-01-05 CO RADIAL Kappa list = 15-Nov-94 Channel list =24-May-01 Calculated as: Elements Spectral impurity data: CAL.909 Teflon(7/94) X-ray path = Vacuum Film type = No supporting film Case number =0 Known Area, % Rest, Diluent/Sample and Mass/Area Eff. Diam. = 25.00 mmEff. Area = 490.6 mm2 KnownConc = 0% Rest = 0% Dil/Sample = 0 ViewedMass = 18000.00 mg Sample Height = 5 mm < means that the concentrationis < 20 ppm <2e means wt % < 2 StdErr. The + in Z + El means involved inSum = 100% Z wt % StdErr Z wt % StdErr Z wt % StdErr Sum Be . . . F 00.88 29 Cu < 51 Sb < 11 + Na 0.043 0.009 30 Zn < 52 Te < 12 Mg < 31 Ga <53 I < 13 + Al 3.71 0.09 32 Ge < 55 Cs < 14 + Si 0.18 0.01 33 As < 56 Ba< 15 + P 0.0037 0.0004 34 Se < Sum La . . . Lu 0.02 10.20 16 S 35 Br <72 Hf <2e 0.006 16 + So < 37 Rb < 73 Ta < 17 + Cl 0.0034 0.0007 38 Sr <74 W < 18 + Ar 0.010 0.001 39 Y < 75 Re <2e 0.005 19 K < 40 + Zr 0.0170.001 76 Os < 20 + Ca 0.0087 0.0008 41 Nb < 77 Ir <2e 0.005 21 + Sc0.0033 0.0006 42 Mo < 78 Pt < 22 Ti < 44 Ru <2e 0.002 79 Au < 23 V < 45Rh <2e 0.002 80 Hg <2e 0.004 24 + Cr < 46 Pd < 81 Tl < 25 + Mn 0.00810.0007 47 Ag < 82 Pb < 26 + Fe 0.13 0.01 48 Cd < 83 Bi < 27 + Co 95.70.1 49 In < 90 Th <2e 0.002 28 + Ni 0.18 0.01 50 Sn < 92 U < LightElements Noble Elements Lanthanides 4 Be 44 Ru <2e 0.002 57 La < 5 B 45Rh <2e 0.002 58 Ce < 6 C 46 Pd < 59 Pr < 7 N 47 Ag < 60 Nd < 8 O 75 Re<2e 0.005 62 Sm < 9 + F < 76 Os < 63 + Eu 0.008 0.002 77 Ir <2e 0.00564 + Gd 0.011 0.003 78 Pt < 65 Tb < 79 Au < 66 Dy < 67 + Ho < 68 + Er <69 Tm < 70 + Yb < 71 + Lu < KnownConc = 0 REST = 0 D/S = 0

[0422] TABLE 18 Quantum Catalytics, LLC ANALYSIS REPORT by UniquantOLD.330 of 4-Jun-01 Today 4-Jun-01 Spectrometers configuration: ARL 8410Rh 60 kV LiF220 LiF420 Ge111 TlAP Sample ident = 14-01-06 Cu/Ag/Au AxTOP Further info = 14-01-06 Cu/Ag/Au AXIAL TOP 6/4/01 Kappa list =15-Nov-94 Channel list = 4-Jun-01 Calculated as: Elements Spectralimpurity data: CAL.909 Teflon (7/94) X-ray path = Vacuum Film type = Nosupporting film Case number = 0 Known Area, % Rest, Diluent/Sample andMass/Area Eff. Diam. = 25.00 mm Eff. Area = 490.6 mm2 KnownConc = 0%Rest = 0% Dil/Sample = 0 Viewed Mass = 18000.00 mg Sample Height = 5 mm< means that the concentration is < 20 ppm <2e means wt % < 2 StdErr.The + in Z + El means involved in Sum = 100% Z wt % StdErr Z wt % StdErrZ wt % StdErr Sum Be . . . F 0 0.41 29 + Cu 96.97 0.09 51 Sb < 11 + Na0.056 0.010 30 + Zn < 52 Te < 12 Mg < 31 + Ga 0.007 0.003 53 I < 13 + Al0.013 0.003 32 Ge < 55 Cs < 14 Si < 33 As < 56 Ba < 15 + P < 34 + Se <Sum La . . . Lu 0.012 0.071 16 + S 0.0032 0.0004 35 + Br < 72 + Hf < 16So 37 + Rb < 73 + Ta < 17 + Cl 0.020 0.002 38 Sr < 74 W < 18 + Ar 0.0110.002 39 Y < 75 + Re 0.021 0.008 19 K < 40 + Zr 0.0074 0.0010 76 Os <20 + Ca 0.0029 0.0008 41 Nb < 77 + Ir 0.026 0.008 21 + Sc < 42 Mo <2e0.002 78 Pt < 22 Ti < 44 Ru < 79 + Au 1.37 0.05 23 V < 45 Rh < 80 Hg <2e0.006 24 Cr < 46 Pd < 81 Tl < 25 Mn < 47 + Ag 1.49 0.06 82 Pb < 26 Fe <48 Cd < 83 Bi < 27 Co < 49 In < 90 Th <2e 0.003 28 Ni < 50 + Sn < 92 U <Light Elements Noble Elements Lanthanides 4 Be 44 Ru < 57 + La <2e 0.0045 B 45 Rh < 58 Ce < 6 C 46 Pd < 59 Pr < 7 N 47 + Ag 1.49 0.06 60 Nd < 8O 75 + Re 0.021 0.008 62 Sm < 9 F < 76 Os < 63 Eu <2e 0.002 77 + Ir0.026 0.008 64 Gd < 78 Pt < 65 Tb <2e 0.002 79 + Au 1.37 0.05 66 Dy < 67Ho < 68 Er < 69 Tm < 70 Yb < 71 + Lu < KnownConc = 0 REST = 0 D/S = 0

[0423] TABLE 19 Quantum Catalytics, LLC ANALYSIS REPORT by UniquantOLD.331 of 4-Jun-01 Today 4-Jun-01 Spectrometers configuration: ARL 8410Rh 60 kV LiF220 LiF420 Ge111 TlAP Sample ident = 14-01-06 Cu/Ag/AuRADIAL Further info = 14-01-06 Cu/Ag/Au RADIAL 06/4/01 Kappa list =15-Nov-94 Channel list = 4-Jun-01 Calculated as: Elements Spectralimpurity data: CAL.909 Teflon (7/94) X-ray path = Vacuum Film type = Nosupporting film Case number = 0 Known Area, % Rest, Diluent/Sample andMass/Area Eff. Diam. = 25.00 mm Eff. Area = 490.6 mm2 KnownConc = 0%Rest = 0% Dil/Sample = 0 Viewed Mass = 18000.00 mg Sample Height = 5 mm< means that the concentration is < 20 ppm <2e means wt % < 2 StdErr.The + in Z + El means involved in Sum = 100% Z wt % StdErr Z wt % StdErrZ wt % StdErr Sum Be . . . F 0 0.040 29 + Cu 97.04 0.08 51 Sb < 11 + Na0.045 0.010 30 + Zn < 52 Te < 12 Mg <2e 0.004 31 Ga <2e 0.003 53 I <13 + Al 0.047 0.004 32 Ge <2e 0.002 55 Cs <2e 0.003 14 Si <2e 0.005 33As < 56 Ba <2e 0.003 15 + P < 34 + Se < Sum La . . . Lu 0.003 0.071 16 +S 0.0066 0.0006 35 + Br < 72 + Hf < 16 So 37 + Rb < 73 + Ta < 17 + Cl0.025 0.002 38 Sr < 74 W < 18 + Ar 0.011 0.002 39 Y < 75 Re <2e 0.00819 + K 0.0021 0.0008 40 + Zr 0.008 0.001 76 Os < 20 + Ca 0.0060 0.000941 Nb < 77 + Ir 0.033 0.008 21 Sc < 42 Mo < 78 Pt < 22 Ti < 44 Ru < 79 +Au 1.33 0.05 23 V < 45 Rh < 80 Hg <2e 0.006 24 + Cr < 46 Pd < 81 Tl < 25Mn < 47 + Ag 1.44 0.05 82 Pb < 26 Fe < 48 Cd < 83 Bi < 27 Co < 49 In <90 Th < 28 Ni < 50 + Sn < 92 U < Light Elements Noble ElementsLanthanides 4 Be 44 Ru < 57 La < 5 B 45 Rh < 58 Ce < 6 C 46 Pd < 59 Pr <7 N 47 + Ag 1.44 0.05 60 Nd < 8 O 75 Re <2e 0.008 62 Sm < 9 F < 76 Os <63 Eu < 77 + Ir 0.033 0.008 64 Gd < 78 Pt < 65 Tb <2e 0.002 79 + Au 1.330.05 66 Dy < 67 Ho < 68 Er < 69 Tm < 70 Yb < 71 + Lu < KnownConc = 0REST = 0 D/S = 0

[0424] TABLE 20 Quantum Catalytics, LLC ANALYSIS REPORT by UniquantOLD.336 of 11-Jun-01 Today 11-Jun-01 Spectrometers configuration: ARL8410 Rh 60 kV LiF220 LiF420 Ge111 TlAP Sample ident = 14-01-07 AXIALFurther info = 14-01-07 AXIAL LEAD TIN ZINC 6/11 CASS 8 Kappa list =15-Nov-94 Channel list = 4-Jun-01 Calculated as: Elements Spectralimpurity data: CAL.909 Teflon (7/94) X-ray path = Vacuum Film type = Nosupporting film Case number = 0 Known Area, % Rest, Diluent/Sample andMass/Area Eff. Diam. = 25.00 mm Eff. Area = 490.6 mm2 KnownConc = 0%Rest = 0% Dil/Sample = 0 Viewed Mass = 18000.00 mg Sample Height = 5 mm< means that the concentration is < 20 ppm <2e means wt % < 2 StdErr.The + in Z + El means involved in Sum = 100% Z wt % StdErr Z wt % StdErrZ wt % StdErr Sum Be . . . F 0 0.051 29 + Cu 0.24 0.02 51 + Sb 0.0230.006 11 + Na < 30 + Zn 25.4 0.2 52 Te < 12 + Mg 0.016 0.008 31 + Ga <53 + I <2e 0.82 13 + Al 2.08 0.07 32 Ge < 55 Cs < 14 + Si 0.018 0.004 33As < 56 Ba < 15 + P < 34 Se < Sum La . . . Lu 0.035 0.072 16 S 35 Br <2e0.001 72 Hf < 16 + So 0.038 0.003 37 + Rb < 73 + Ta < 17 + Cl 0.0530.004 38 Sr < 74 + W <2e 0.012 18 Ar < 39 + Y <2e 0.002 75 Re < 19 K <40 + Zr 0.024 0.005 76 + Os < 20 + Ca <2e 0.031 41 Nb < 77 + Ir < 21 Sc< 42 Mo < 78 + Pt < 22 Ti < 44 + Ru <2e 0.005 79 Au < 23 V < 45 Rh < 80Hg < 24 Cr < 46 Pd < 81 + Tl < 25 Mn < 47 Ag < 82 + Pb 16.9 0.2 26 Fe <48 + Cd 0.014 0.005 83 + Bi < 27 Co <2e 0.001 49 + In <2e 0.011 90 + Th< 28 + Ni 0.007 0.003 50 + Sn 54.7 0.2 92 U < Light Elements NobleElements Lanthanides 4 Be 44 + Ru <2e 0.005 57 La < 5 B 45 Rh < 58 + Ce0.030 0.010 6 C 46 Pd < 59 Pr <2e 0.006 7 N 47 Ag < 60 + Nd <2e 0.004 8O 75 Re < 62 Sm < 9 F < 76 + Os < 63 Eu < 77 + Ir < 64 Gd < 78 + Pt < 65Tb < 79 Au < 66 Dy < 67 Ho < 68 Er < 69 Tm < 70 Yb < 71 Lu < KnownConc =0 REST = 0 D/S = 0

[0425] TABLE 21 Quantum Catalytics, LLC ANALYSIS REPORT by UniquantOLD.337 of 4-Jun-01 Today 11-Jun-01 Spectrometers configuration: ARL8410 Rh 60 kV LiF220 LiF420 Ge111 TlAP Sample ident = 14-01-07 RADIALFurther info = 14-01-07 RADIAL LEAD/TIN/ZINC 6/11 CS 8 Kappa list =15-Nov-94 Channel list = 4-Jun-01 Calculated as: Elements Spectralimpurity data: CAL.909 Teflon (7/94) X-ray path = Vacuum Film type = Nosupporting film Case number = 0 Known Area, % Rest, Diluent/Sample andMass/Area Eff. Diam. = 25.00 mm Eff. Area = 490.6 mm2 KnownConc = 0%Rest = 0% Dil/Sample = 0 Viewed Mass = 18000.00 mg Sample Height = 5 mm< means that the concentration is < 20 ppm <2e means wt % < 2 StdErr.The + in Z + El means involved in Sum = 100% Z wt % StdErr Z wt % StdErrZ wt % StdErr Sum Be . . . F 0 0.046 29 + Cu 0.014 0.002 51 + Sb 0.0150.005 11 + Na < 30 + Zn 33.2 0.2 52 Te < 12 + Mg < 31 + Ga < 53 + I <2e0.72 13 + Al 0.17 0.01 32 Ge < 55 Cs < 14 + Si 0.026 0.004 33 As < 56 Ba< 15 P < 34 Se < Sum La . . . Lu 0.031 0.069 16 S 35 Br < 72 Hf < 16 +So < 37 + Rb < 73 Ta < 17 + Cl 0.031 0.003 38 Sr < 74 + W 0.033 0.014 18Ar < 39 + Y < 75 Re < 19 K < 40 + Zr 0.016 0.005 76 + Os < 20 + Ca <2e0.027 41 Nb < 77 + Ir < 21 Sc < 42 Mo < 78 + Pt < 22 Ti < 44 + Ru 0.0110.005 79 Au < 23 V < 45 Rh < 80 Hg < 24 Cr < 46 Pd < 81 + Tl <2e 0.01425 Mn < 47 Ag < 82 + Pb 18.3 0.2 26 Fe < 48 + Cd 0.025 0.004 83 Bi < 27Co < 49 + In <2e 0.010 90 Th < 28 Ni < 50 + Sn 47.9 0.2 92 U < LightElements Noble Elements Lanthanides 4 Be 44 + Ru 0.011 0.005 57 La <2e0.008 5 B 45 Rh < 58 + Ce <2e 0.010 6 C 46 Pd < 59 Pr < 7 N 47 Ag < 60Nd < 8 O 75 Re < 62 Sm < 9 F < 76 + Os < 63 Eu < 77 + Ir < 64 Gd <2e0.004 78 + Pt < 65 Tb < 79 Au < 66 Dy < 67 + Ho 0.012 0.006 68 Er <2e0.004 69 Tm <2e 0.004 70 Yb <2e 0.004 71 Lu < KnownConc = 0 REST = 0 D/S= 0

[0426] TABLE 22 Quantum Catalytics, LLC ANALYSIS REPORT by UniquantOLD.342 of 14-Jun-01 Today 14-Jun-01 Spectrometers configuration: ARL8410 Rh 60 kV LiF220 LiF420 Ge111 TlAP Sample ident = 14-01-08 AXIALFurther info = 14-01-08 AXIAL Sn, K, Na, Mg 6/14 Kappa list = 15-Nov-94Channel list = 4-Jun-01 Calculated as: Elements Spectral impurity data:CAL.909 Teflon (7/94) X-ray path = Vacuum Film type = No supporting filmCase number = 0 Known Area, % Rest, Diluent/Sample and Mass/Area Eff.Diam. = 25.00 mm Eff. Area = 490.6 mm2 KnownConc = 0% Rest = 0%Dil/Sample = 0 Viewed Mass = 18000.00 mg Sample Height = 5 mm < meansthat the concentration is < 20 ppm <2e means wt % < 2 StdErr. The + inZ + El means involved in Sum = 100% Z wt % StdErr Z wt % StdErr Z wt %StdErr Sum Be . . . F 0 0.060 29 + Cu 0.079 0.006 51 Sb < 11 + Na 1.070.05 30 Zn < 52 Te < 12 + Mg 0.85 0.04 31 Ga < 53 + I <2e 1.43 13 + Al1.53 0.06 32 Ge < 55 Cs < 14 + Si 0.16 0.01 33 As < 56 Ba < 15 + P < 34Se < Sum La . . . Lu 0.021 0.072 16 S 35 Br < 72 Hf <2e 0.003 16 + So0.044 0.004 37 Rb < 73 Ta < 17 + Cl 0.015 0.001 38 + Sr < 74 + W 0.0310.004 18 Ar < 39 Y < 75 Re < 19 K < 40 + Zr 0.047 0.004 76 Os < 20 + Ca< 41 + Nb < 77 + Ir <2e 0.003 21 + Sc 0.007 0.002 42 Mo < 78 Pt < 22 Ti< 44 + Ru < 79 Au < 23 V <2e 0.002 45 Rh < 80 Hg < 24 Cr < 46 Pd < 81 Tl< 25 Mn < 47 Ag < 82 + Pb 0.067 0.006 26 + Fe 0.017 0.002 48 + Cd 0.0410.005 83 Bi <2e 0.002 27 + Co 0.003 0.001 49 + In <2e 0.019 90 + Th <28 + Ni 0.021 0.002 50 + Sn 95.6 0.1 92 U < Light Elements NobleElements Lanthanides 4 Be 44 + Ru < 57 La < 5 B 45 Rh < 58 Ce <2e 0.0076 C 46 Pd < 59 Pr < 7 N 47 Ag < 60 Nd <2e 0.005 8 O 75 Re < 62 Sm < 9 F< 76 Os < 63 Eu < 77 + Ir <2e 0.003 64 Gd < 78 Pt < 65 Tb < 79 Au < 66Dy < 67 Ho <2e 0.005 68 Er < 69 Tm <2e 0.004 70 Yb < 71 Lu < KnownConc =0 REST = 0 D/S = 0

[0427] TABLE 23 Quantum Catalytics, LLC ANALYSIS REPORT by UniquantOLD.343 of 4-Jun-01 Today 14-Jun-01 Spectrometers configuration: ARL8410 Rh 60 kV LiF220 LiF420 Ge111 TlAP Sample ident = 14-01-08 RADIALFurther info = 14-01-08 RADIAL Sn, K, Na, Mg 6/14 Kappa list = 15-Nov-94Channel list = 4-Jun-01 Calculated as: Elements Spectral impurity data:CAL.909 Teflon (7/94) X-ray path = Vacuum Film type = No supporting filmCase number = 0 Known Area, % Rest, Diluent/Sample and Mass/Area Eff.Diam. = 25.00 mm Eff. Area = 490.6 mm2 KnownConc = 0% Rest = 0%Dil/Sample = 0 Viewed Mass = 18000.00 mg Sample Height = 5 mm < meansthat the concentration is < 20 ppm <2e means wt % < 2 StdErr. The + inZ + El means involved in Sum = 100% Z wt % StdErr Z wt % StdErr Z wt %StdErr Sum Be . . . F 0 0.056 29 + Cu 0.14 0.01 51 Sb < 11 + Na 2.820.08 30 + Zn 0.003 0.002 52 Te < 12 + Mg 1.04 0.04 31 Ga < 53 + I <2e1.40 13 + Al 1.69 0.06 32 Ge < 55 Cs < 14 + Si 0.29 0.02 33 As < 56 Ba <15 + P 0.0022 0.0004 34 Se < Sum La . . . Lu 0.025 0.065 16 S 35 Br < 72Hf <2e 0.003 16 + So 0.032 0.003 37 Rb < 73 Ta < 17 + Cl 0.013 0.001 38Sr < 74 + W 0.048 0.004 18 Ar < 39 Y < 75 Re < 19 K < 40 + Zr 0.0430.004 76 Os <2e 0.003 20 + Ca < 41 + Nb < 77 + Ir <2e 0.003 21 Sc <2e0.002 42 Mo < 78 Pt < 22 Ti < 44 + Ru < 79 Au < 23 V <2e 0.001 45 Rh <80 Hg < 24 Cr <2e 0.002 46 Pd < 81 + Tl 0.006 0.003 25 Mn <2e 0.001 47Ag < 82 + Pb 0.069 0.006 26 + Fe 0.023 0.002 48 + Cd 0.029 0.006 83 Bi<2e 0.002 27 Co <2e 0.001 49 + In <2e 0.019 90 + Th < 28 + Ni 0.0450.004 50 + Sn 93.6 0.1 92 U < Light Elements Noble Elements Lanthanides4 Be 44 + Ru < 57 La < 5 B 45 Rh < 58 Ce <2e 0.006 6 C 46 Pd < 59 Pr < 7N 47 Ag < 60 Nd <2e 0.004 8 O 75 Re < 62 Sm <2e 0.005 9 F < 76 Os <2e0.003 63 Eu <2e 0.004 77 + Ir <2e 0.003 64 Gd < 78 Pt < 65 Tb < 79 Au <66 Dy < 67 Ho < 68 Er < 69 Tm < 70 Yb < 71 Lu < KnownConc = 0 REST = 0D/S = 0

[0428] TABLE 24 Quantum Catalytics, LLC ANALYSIS REPORT by UniquantOLD.314 of 24-May-01 Today 24-May-01 Spectrometers configuration: ARL8410 Rh 60 kV LiF220 LiF420 Ge111 TlAP Sample ident = 15-01-01 Si AXIALBLK Further info = 15-01-01 Si AXIAL BLK 5/24 Kappa list = 15-Nov-94Channel list = 24-May-01 Calculated as: Elements Spectral impurity data:CAL.909 Teflon (7/94) X-ray path = Vacuum Film type = No supporting filmCase number = 0 Known Area, % Rest, Diluent/Sample and Mass/Area Eff.Diam. = 25.00 mm Eff. Area = 490.6 mm2 KnownConc = 0% Rest = 0%Dil/Sample = 0 Viewed Mass = 18000.00 mg Sample Height = 5 mm < meansthat the concentration is < 20 ppm <2e means wt % < 2 StdErr. The + inZ + El means involved in Sum = 100% Z wt % StdErr Z wt % StdErr Z wt %StdErr Sum Be . . . F 0.059 0.021 29 + Cu 0.012 0.001 51 Sb < 11 + Na0.004 0.002 30 + Zn 0.0021 0.0005 52 Te < 12 Mg < 31 + Ga 0.0038 0.000553 I < 13 + Al 1.18 0.05 32 Ge < 55 + Cs <2e 0.003 14 + Si 98.58 0.06 33As < 56 + Ba 0.008 0.003 15 + P 0.013 0.001 34 Se < Sum La . . . Lu0.004 0.018 16 + S 0.013 0.001 35 Br < 72 Hf < 16 So 37 Rb < 73 Ta <17 + Cl 0.004 0.002 38 Sr < 74 + W 0.007 0.001 18 + Ar 0.013 0.003 39 Y< 75 Re < 19 + K < 40 + Zr < 76 Os < 20 + Ca 0.0092 0.0009 41 Nb < 77 Ir< 21 Sc < 42 Mo < 78 Pt < 22 + Ti 0.019 0.002 44 Ru < 79 Au < 23 V < 45Rh < 80 Hg < 24 + Cr 0.0031 0.0005 46 Pd < 81 Tl < 25 + Mn < 47 Ag < 82Pb < 26 + Fe 0.055 0.005 48 Cd < 83 Bi < 27 Co < 49 In < 90 Th < 28 + Ni0.0051 0.0006 50 Sn < 92 U < Light Elements Noble Elements Lanthanides 4Be 44 Ru < 57 La < 5 B 45 Rh < 58 Ce < 6 C 46 Pd < 59 Pr < 7 N 47 Ag <60 Nd < 8 O 75 Re < 62 Sm < 9 + F 0.059 0.021 76 Os < 63 Eu < 77 Ir < 64Gd < 78 Pt < 65 Tb < 79 Au < 66 Dy < 67 Ho < 68 Er < 69 Tm < 70 Yb < 71Lu < KnownConc = 0 REST = 0 D/S = 0

[0429] TABLE 25 Quantum Catalytics, LLC ANALYSIS REPORT OLD.317 of24-May-01 Today 24-May- Spectrometers configuration: ARL 8410 Rh 60 kVLiF220 LiF420 Ge111 TlAP Sample ident = 15-01-01 Si RADIAL BLK Furtherinfo = 15-01-01 Si RADIAL BLK 5/24 Kappa list = 15-Nov-94 Channel list =24-May-01 Calculated as: Elements Spectral impurity data: CAL.909 Teflon(7/94) X-ray path = Vacuum Film type = No supporting film Case number =0 Known Area, % Rest, Diluent/Sample and Mass/Area Eff. Diam. = 25.00 mmEff. Area = 490.6 mm2 KnownConc = 0% Rest = 0% Dil/Sample = 0 ViewedMass = 18000.00 mg Sample Height = 5 mm < means that the concentrationis < 20 ppm <2e means wt % < 2 StdErr. The + in Z + El means involved inSum = 100% Z wt % StdErr Z wt % StdErr Z wt % StdErr Sum Be . . . F 00.021 29 + Cu 0.0101 0.0009 51 Sb < 11 + Na 0.016 0.002 30 + Zn 0.00200.0005 52 Te < 12 Mg < 31 + Ga 0.0043 0.0005 53 I < 13 + Al 1.46 0.05 32Ge < 55 + Cs <2e 0.003 14 + Si 98.12 0.07 33 As < 56 + Ba <2e 0.003 15 +P 0.018 0.002 34 Se < Sum La . . . Lu 0.005 0.020 16 S 35 Br < 72 + Hf0.003 0.001 16 + So 0.14 0.01 37 Rb < 73 Ta < 17 + Cl 0.019 0.002 38 Sr< 74 + W 0.011 0.001 18 + Ar 0.012 0.003 39 Y < 75 Re < 19 + K 0.0140.001 40 + Zr < 76 Os < 20 + Ca 0.077 0.006 41 Nb < 77 + Ir < 21 Sc < 42Mo < 78 Pt < 22 + Ti 0.029 0.003 44 Ru < 79 Au < 23 + V < 45 Rh < 80 Hg< 24 + Cr 0.0026 0.0005 46 Pd < 81 Tl < 25 Mn < 47 Ag < 82 Pb < 26 + Fe0.042 0.004 48 Cd < 83 Bi < 27 Co < 49 In < 90 Th < 28 + Ni 0.00530.0006 50 Sn < 92 U < Light Elements Noble Elements Lanthanides 4 Be 44Ru < 57 La < 5 B 45 Rh < 58 Ce < 6 C 46 Pd < 59 Pr < 7 N 47 Ag < 60 Nd <8 O 75 Re < 62 Sm < 9 F < 76 Os < 63 Eu < 77 + Ir < 64 Gd <2e 0.001 78Pt < 65 Tb < 79 Au < 66 Dy < 67 Ho < 68 Er < 69 Tm < 70 Yb < 71 Lu <KnownConc = 0 REST = 0 D/S = 0

[0430] TABLE 26 Quantum Catalytics, LLC ANALYSIS REPORT by UniquantOLD.237 of 23-Apr-01 Today 23-Apr-01 Spectrometers configuration: ARL8410 Rh 60 kV LiF220 LiF420 Ge111 TlAP Sample ident = 15-01-01 SiSECTION TOP Further info = 15-01-01 Si MID SECTION TOP FACE AXIAL Kappalist = 15-Nov-94 Channel list = 19-Apr-01 Calculated as: ElementsSpectral impurity data: CAL.909 Teflon (7/94) X-ray path = Vacuum Filmtype = No supporting film Case number = 0 Known Area, % Rest,Diluent/Sample and Mass/Area Eff. Diam. = 25.00 mm Eff. Area = 490.6 mm2KnownConc = 0% Rest = 0% Dil/Sample = 0 Viewed Mass = 18000.00 mg SampleHeight = 5 mm < means that the concentration is < 20 ppm <2e means wt %< 2 StdErr. The + in Z + El means involved in Sum = 100% Z wt % StdErr Zwt % StdErr Z wt % StdErr Sum Be . . . F 0 0.018 29 + Cu 0.0070 0.000651 Sb < 11 + Na 0.050 0.004 30 + Zn 0.0033 0.0005 52 Te < 12 Mg < 31 +Ga 0.0020 0.0004 53 I < 13 + Al 1.02 0.04 32 Ge < 55 Cs <2e 0.003 14 +Si 98.48 0.06 33 As < 56 + Ba <2e 0.003 15 + P 0.019 0.002 34 Se < SumLa . . . Lu 0.002 0.018 16 + S 0.14 0.01 35 Br < 72 Hf < 16 So 37 Rb <73 Ta < 17 + Cl 0.075 0.006 38 Sr < 74 + W 0.009 0.001 18 + Ar 0.0120.003 39 Y < 75 Re < 19 + K 0.028 0.002 40 + Zr < 76 Os < 20 + Ca 0.0250.002 41 Nb < 77 Ir < 21 Sc < 42 Mo < 78 Pt < 22 + Ti 0.064 0.005 44 Ru< 79 Au < 23 + V < 45 Rh < 80 Hg < 24 + Cr < 46 Pd < 81 Tl < 25 Mn < 47Ag < 82 Pb < 26 + Fe 0.045 0.004 48 + Cd < 83 Bi < 27 + Co < 49 In <90 + Th <2e 0.001 28 + Ni 0.0051 0.0006 50 Sn < 92 U < Light ElementsNoble Elements Lanthanides 4 Be 44 Ru < 57 La < 5 B 45 Rh < 58 Ce < 6 C46 Pd < 59 Pr < 7 N 47 Ag < 60 Nd < 8 O 75 Re < 62 Sm < 9 F < 76 Os < 63Eu < 77 Ir < 64 Gd < 78 Pt < 65 Tb < 79 Au < 66 Dy < 67 Ho < 68 Er < 69Tm < 70 Yb < 71 Lu < KnownConc = 0 REST = 0 D/S = 0

[0431] TABLE 27 Quantum Catalytics, LLC ANALYSIS REPORT by UniquantOLD.245 of 19-Apr-01 Today 24-Apr-01 Spectrometers configuration: ARL8410 Rh 60 kV LiF220 LiF420 Ge111 TlAP Sample ident = 15-01-01 MIDBOTTOM FACE Further info = 15-01-01 Si MID SECTION BOT FACE AXIAL Kappalist = 15-Nov-94 Channel list = 19-Apr-01 Calculated as: ElementsSpectral impurity data: CAL.909 Teflon (7/94) X-ray path = Vacuum Filmtype = No supporting film Case number = 0 Known Area, % Rest,Diluent/Sample and Mass/Area Eff. Diam. = 25.00 mm Eff. Area = 490.6 mm2KnownConc = 0% Rest = 0% Dil/Sample = 0 Viewed Mass = 18000.00 mg SampleHeight = 5 mm < means that the concentration is < 20 ppm <2e means wt %< 2 StdErr. The + in Z + El means involved in Sum = 100% Z wt % StdErr Zwt % StdErr Z wt % StdErr Sum Be . . . F 0 0.017 29 + Cu 0.0075 0.000751 Sb < 11 + Na 0.033 0.003 30 + Zn < 52 Te < 12 Mg < 31 + Ga 0.00210.0003 53 I < 13 + Al 0.71 0.04 32 Ge < 55 + Cs <2e 0.002 14 + Si 98.810.05 33 As < 56 + Ba <2e 0.003 15 + P 0.016 0.001 34 Se < Sum La . . .Lu 0.006 0.018 16 + S 0.23 0.02 35 Br < 72 Hf < 16 So 37 Rb < 73 Ta <17 + Cl 0.057 0.005 38 Sr < 74 + W 0.007 0.001 18 + Ar 0.007 0.002 39 Y< 75 Re < 19 + K 0.012 0.001 40 Zr < 76 Os < 20 + Ca 0.041 0.003 41 Nb <77 Ir < 21 Sc < 42 Mo < 78 Pt < 22 + Ti 0.020 0.002 44 Ru < 79 Au < 23 +V < 45 Rh < 80 Hg < 24 + Cr < 46 Pd < 81 Tl < 25 Mn < 47 Ag < 82 Pb <26 + Fe 0.026 0.002 48 Cd < 83 Bi < 27 + Co < 49 In < 90 Th < 28 + Ni0.0034 0.0006 50 Sn < 92 U < Light Elements Noble Elements Lanthanides 4Be 44 Ru < 57 La < 5 B 45 Rh < 58 Ce < 6 C 46 Pd < 59 Pr < 7 N 47 Ag <60 Nd < 8 O 75 Re < 62 Sm < 9 F < 76 Os < 63 Eu < 77 Ir < 64 Gd < 78 Pt< 65 Tb < 79 Au < 66 Dy < 67 Ho <2e 0.002 68 + Er <2e 0.001 69 Tm < 70Yb < 71 Lu < KnownConc = 0 REST = 0 D/S = 0

[0432] TABLE 28 Quantum Catalytics, LLC ANALYSIS REPORT by UniquantOLD.326 of 1-Jun-01 Today 4-Jun-01 Spectrometers configuration: ARL 8410Rh 60 kV LiF220 LiF420 Ge111 TlAP Sample ident = 15-01-02 AXIAL TOPFurther info = 15-01-02 AXIAL TOP Kappa list = 15-Nov-94 Channel list =24-May-01 Calculated as: Elements Spectral impurity data: CAL.909 Teflon(7/94) X-ray path = Vacuum Film type = No supporting film Case number =0 Known Area, % Rest, Diluent/Sample and Mass/Area Eff. Diam. = 25.00 mmEff. Area = 490.6 mm2 KnownConc = 0% Rest = 0% Dil/Sample = 0 ViewedMass = 18000.00 mg Sample Height = 5 mm < means that the concentrationis < 20 ppm <2e means wt % < 2 StdErr. The + in Z + El means involved inSum = 100% Z wt % StdErr Z wt % StdErr Z wt % StdErr Sum Be . . . F 00.026 29 + Cu 0.012 0.002 51 Sb < 11 Na <2e 0.009 30 Zn < 52 Te < 12 Mg< 31 Ga < 53 I < 13 + Al 1.89 0.06 32 Ge < 55 Cs < 14 + Si 0.032 0.00533 As < 56 Ba <2e 0.003 15 + P 0.0033 0.0003 34 Se < Sum La . . . Lu 00.20 16 S 35 Br < 72 Hf <2e 0.005 16 + So 0.0077 0.0007 37 Rb < 73 Ta <17 + Cl 0.0040 0.0006 38 Sr < 74 + W 0.009 0.004 18 + Ar 0.012 0.001 39Y < 75 Re <2e 0.004 19 K < 40 + Zr 0.0099 0.0009 76 Os < 20 + Ca 0.00530.0006 41 Nb < 77 Ir < 21 + Sc 0.0025 0.0005 42 Mo < 78 Pt < 22 Ti < 44Ru < 79 Au < 23 V < 45 Rh < 80 Hg < 24 Cr < 46 Pd < 81 Tl < 25 Mn < 47Ag <2e 0.002 82 Pb < 26 + Fe 98.01 0.07 48 Cd <2e 0.001 83 Bi < 27 Co <49 In < 90 + Th 0.006 0.002 28 Ni < 50 Sn < 92 U < Light Elements NobleElements Lanthanides 4 Be 44 Ru < 57 La < 5 B 45 Rh < 58 Ce < 6 C 46 Pd< 59 + Pr <2e 0.006 7 N 47 Ag <2e 0.002 60 Nd < 8 O 75 Re <2e 0.004 62 +Sm < 9 F < 76 Os < 63 Eu < 77 Ir < 64 Gd < 78 Pt < 65 + Tb < 79 Au < 66Dy < 67 Ho < 68 + Er < 69 + Tm < 70 Yb < 71 Lu < KnownConc = 0 REST = 0D/S = 0

[0433] TABLE 29 Quantum Catalytics, LLC ANALYSIS REPORT by UniquantOLD.329 of 1-Jun-01 Today 4-Jun-01 Spectrometers configuration: ARL 8410Rh 60 kV LiF220 LiF420 Ge111 TlAP Sample ident = 15-01-02 Fe RADIALFurther info = 15-01-02 Fe RADIAL Kappa list = 15-Nov-94 Channel list =24-May-01 Calculated as: Elements Spectral impurity data: CAL.909 Teflon(7/94) X-ray path = Vacuum Film type = No supporting film Case number =0 Known Area, % Rest, Diluent/Sample and Mass/Area Eff. Diam. = 25.00 mmEff. Area = 490.6 mm2 KnownConc = 0% Rest = 0% Dil/Sample = 0 ViewedMass = 18000.00 mg Sample Height = 5 mm < means that the concentrationis < 20 ppm <2e means wt % < 2 StdErr. The + in Z + El means involved inSum = 100% Z wt % StdErr Z wt % StdErr Z wt % StdErr Sum Be . . . F 00.024 29 + Cu 0.014 0.002 51 Sb < 11 + Na 0.040 0.009 30 Zn < 52 Te < 12Mg < 31 Ga < 53 I < 13 + Al 2.96 0.08 32 Ge < 55 Cs < 14 + Si 0.14 0.0133 As < 56 Ba < 15 + P 0.0036 0.0003 34 Se < Sum La . . . Lu 0 0.20 16 S35 Br < 72 Hf < 16 + So 0.012 0.001 37 Rb < 73 Ta < 17 + Cl 0.00440.0006 38 Sr < 74 W < 18 + Ar 0.013 0.001 39 Y < 75 Re <2e 0.004 19 K <40 + Zr 0.012 0.001 76 Os < 20 + Ca 0.0073 0.0007 41 Nb < 77 Ir < 21 +Sc 0.0026 0.0005 42 Mo < 78 Pt < 22 Ti < 44 Ru < 79 Au < 23 V < 45 Rh <80 Hg <2e 0.003 24 Cr < 46 Pd < 81 Tl < 25 Mn < 47 Ag < 82 Pb < 26 + Fe96.78 0.09 48 Cd < 83 Bi < 27 Co < 49 In < 90 Th <2e 0.002 28 Ni < 50 Sn< 92 U < Light Elements Noble Elements Lanthanides 4 Be 44 Ru < 57 La <5 B 45 Rh < 58 Ce <2e 0.003 6 C 46 Pd < 59 Pr < 7 N 47 Ag < 60 Nd < 8 O75 Re <2e 0.004 62 + Sm < 9 F < 76 Os < 63 Eu <2e 0.003 77 Ir < 64 Gd <78 Pt < 65 + Tb < 79 Au < 66 Dy < 67 Ho < 68 + Er < 69 + Tm < 70 Yb < 71Lu < KnownConc = 0 REST = 0 D/S = 0

[0434] TABLE 30 Quantum Catalytics, LLC ANALYSIS REPORT by UniquantOLD.338 of 11-Jun-01 Today 11-Jun-01 Spectrometers configuration: ARL8410 Rh 60 kV LiF220 LiF420 Ge111 TlAP Sample ident = 15-01-04 AXIALFurther info = 15-01-04 Ni/W/Ta/Hf AXIAL 6/11 Kappa list = 15-Nov-94Channel list = 4-Jun-01 Calculated as: Elements Spectral impurity data:CAL.909 Teflon (7/94) X-ray path = Vacuum Film type = No supporting filmCase number = 0 Known Area, % Rest, Diluent/Sample and Mass/Area Eff.Diam. = 25.00 mm Eff. Area = 490.6 mm2 KnownConc = 0% Rest = 0%Dil/Sample = 0 Viewed Mass = 18000.00 mg Sample Height = 5 mm < meansthat the concentration is < 20 ppm <2e means wt % < 2 StdErr. The + inZ + El means involved in Sum = 100% Z wt % StdErr Z wt % StdErr Z wt %StdErr Sum Be . . . F 0 0.036 29 Cu < 51 Sb < 11 + Na 0.066 0.009 30 Zn< 52 Te < 12 Mg < 31 Ga < 53 I < 13 + Al 3.57 0.09 32 Ge < 55 Cs < 14 +Si 0.23 0.02 33 As < 56 Ba < 15 + P 0.0025 0.0004 34 + Se < Sum La . . .Lu 0.58 1.17 16 + S 0.0069 0.0006 35 Br < 72 + Hf 1.78 0.06 16 So 37 Rb< 73 + Ta 1.76 0.06 17 + Cl 0.0044 0.0008 38 Sr < 74 + W 1.49 0.06 18 +Ar 0.018 0.002 39 Y < 75 Re < 19 K < 40 + Zr < 76 Os < 20 + Ca 0.00250.0008 41 Nb < 77 + Ir < 21 + Sc 0.0036 0.0009 42 Mo < 78 Pt < 22 Ti <44 Ru < 79 Au < 23 V < 45 Rh < 80 + Hg < 24 Cr < 46 Pd < 81 Tl < 25 Mn <47 Ag < 82 Pb < 26 Fe < 48 Cd < 83 + Bi < 27 Co < 49 In < 90 Th <2e0.003 28 + Ni 90.5 0.1 50 Sn < 92 U < Light Elements Noble ElementsLanthanides 4 Be 44 Ru < 57 La < 5 B 45 Rh < 58 Ce < 6 C 46 Pd < 59 Pr <7 N 47 Ag < 60 Nd < 8 O 75 Re < 62 Sm < 9 F < 76 Os < 63 Eu <2e 0.00277 + Ir < 64 Gd < 78 Pt < 65 Tb < 79 Au < 66 Dy < 67 + Ho < 68 + Er <69 + Tm < 70 + Yb 0.58 0.26 71 Lu < KnownConc = 0 REST = 0 D/S = 0

[0435] TABLE 31 Quantum Catalytics, LLC ANALYSIS REPORT by UniquantOLD.339 of 4-Jun-01 Today 11-Jun-01 Spectrometers configuration: ARL8410 Rh 60 kV LiF220 LiF420 Ge111 TlAP Sample ident = 15-01-04 RADIALFurther info = 15-01-04 Ni/W/Ta/Hf RADIAL 6/11 Kappa list = 15-Nov-94Channel list = 4-Jun-01 Calculated as: Elements Spectral impurity data:CAL.909 Teflon (7/94) X-ray path = Vacuum Film type = No supporting filmCase number = 0 Known Area, % Rest, Diluent/Sample and Mass/Area Eff.Diam. = 25.00 mm Eff. Area = 490.6 mm2 KnownConc = 0% Rest = 0%Dil/Sample = 0 Viewed Mass = 18000.00 mg Sample Height = 5 mm < meansthat the concentration is < 20 ppm <2e means wt % < 2 StdErr. The + inZ + El means involved in Sum = 100% Z wt % StdErr Z wt % StdErr Z wt %StdErr Sum Be . . . F 0 0.036 29 + Cu < 51 Sb < 11 + Na 0.043 0.009 30Zn < 52 Te < 12 Mg < 31 + Ga <2e 0.002 53 I < 13 + Al 3.38 0.09 32 + Ge< 55 Cs <2e 0.003 14 + Si 0.74 0.04 33 As < 56 Ba < 15 + P < 34 + Se <Sum La . . . Lu 0.57 1.16 16 + S 0.0053 0.0005 35 Br < 72 + Hf 2.00 0.0716 So 37 Rb < 73 + Ta 1.78 0.06 17 + Cl 0.0059 0.0008 38 Sr < 74 + W1.50 0.06 18 + Ar 0.019 0.002 39 Y < 75 + Re < 19 K < 40 + Zr < 76 Os <20 Ca < 41 Nb < 77 + Ir < 21 + Sc 0.0020 0.0009 42 Mo < 78 Pt < 22 Ti <44 Ru < 79 + Au < 23 V < 45 Rh < 80 + Hg < 24 Cr < 46 Pd < 81 Tl < 25 Mn< 47 Ag < 82 Pb < 26 Fe < 48 Cd <2e 0.002 83 + Bi < 27 Co < 49 In < 90Th <2e 0.003 28 + Ni 90.0 0.2 50 Sn < 92 U < Light Elements NobleElements Lanthanides 4 Be 44 Ru < 57 La < 5 B 45 Rh < 58 Ce < 6 C 46 Pd< 59 Pr < 7 N 47 Ag < 60 Nd < 8 O 75 + Re < 62 Sm < 9 F < 76 Os < 63 Eu< 77 + Ir < 64 Gd <2e 0.002 78 Pt < 65 Tb < 79 + Au < 66 Dy < 67 + Ho <68 + Er < 69 + Tm < 70 + Yb 0.57 0.26 71 Lu < KnownConc = 0 REST = 0 D/S= 0

[0436] TABLE 32 Quantum Catalytics, LLC ANALYSIS REPORT by UniquantOLD.615 of 7-Mar-02 Today 7-Mar-02 Spectrometers configuration: ARL 8410Rh 60 kV LiF220 LiF420 Ge111 TlAP Sample ident = 14-00-01 AX Furtherinfo = 14-00-01 AXIAL POLISHED VAC 3/7/02 Kappa list = 15-Nov-94 Channellist = 8-Jan-02 Calculated as: Elements Spectral impurity data: CAL.909Teflon (7/94) X-ray path = Vacuum Film type = No supporting film Casenumber = 0 Known Area, % Rest, Diluent/Sample and Mass/Area Eff. Diam. =25.00 mm Eff. Area = 490.6 mm2 KnownConc = 0% Rest = 0% Dil/Sample = 0Viewed Mass = 18000.00 mg Sample Height = 5 mm < means that theconcentration is < 20 ppm <2e means wt % < 2 StdErr. The + in Z + Elmeans involved in Sum = 100% Z wt % StdErr Z wt % StdErr Z wt % StdErrSum Be . . . F 0 0.043 29 + Cu 98.88 0.05 51 Sb < 11 + Na 0.063 0.01230 + Zn < 52 Te < 12 Mg < 31 + Ga 0.008 0.003 53 I < 13 + Al 0.33 0.0232 Ge < 55 Cs < 14 + Si 0.66 0.03 33 As < 56 Ba < 15 + P < 34 Se < SumLa . . . Lu 0.021 0.073 16 + S 0.0042 0.0004 35 Br < 72 + Hf < 16 So 37Rb < 73 + Ta < 17 + Cl 0.026 0.002 38 Sr < 74 W < 18 + Ar 0.013 0.001 39Y < 75 Re < 19 K < 40 Zr < 76 Os < 20 Ca < 41 Nb < 77 Ir <2e 0.008 21 +Sc < 42 Mo <2e 0.002 78 Pt < 22 Ti < 44 Ru < 79 Au < 23 V < 45 Rh <2e0.002 80 Hg <2e 0.006 24 Cr < 46 Pd < 81 Tl < 25 Mn < 47 Ag <2e 0.002 82Pb < 26 Fe < 48 Cd <2e 0.002 83 Bi < 27 Co < 49 In < 90 Th < 28 Ni < 50Sn < 92 U < Light Elements Noble Elements Lanthanides 4 Be 44 Ru < 57 +La 0.012 0.005 5 B 45 Rh <2e 0.002 58 Ce < 6 C 46 Pd < 59 Pr < 7 N 47 Ag<2e 0.002 60 Nd < 8 O 75 Re < 62 Sm < 9 F < 76 Os < 63 Eu < 77 Ir <2e0.008 64 Gd < 78 Pt < 65 Tb <2e 0.002 79 Au < 66 Dy < 67 Ho < 68 Er <2e0.004 69 Tm <2e 0.004 70 Yb < 71 + Lu < KnownConc = 0 REST = 0 D/S = 0

[0437] TABLE 33 Quantum Catalytics, LLC ANALYSIS REPORT by UniquantOLD.620 of 8-Jan-02 Today 7-Mar-02 Spectrometers configuration: ARL 8410Rh 60 kV LiF220 LiF420 Ge111 TlAP Sample ident = 14-00-01 RAD Furtherinfo = 14-00-01 RADIAL POLISHED VAC 3/7/02 Kappa list = 15-Nov-94Channel list = 8-Jan-02 Calculated as: Elements Spectral impurity data:CAL.909 Teflon (7/94) X-ray path = Vacuum Film type = No supporting filmCase number = 0 Known Area, % Rest, Diluent/Sample and Mass/Area Eff.Diam. = 25.00 mm Eff. Area = 490.6 mm2 KnownConc = 0% Rest = 0%Dil/Sample = 0 Viewed Mass = 18000.00 mg Sample Height = 5 mm < meansthat the concentration is < 20 ppm <2e means wt % < 2 StdErr. The + inZ + El means involved in Sum = 100% Z wt % StdErr Z wt % StdErr Z wt %StdErr Sum Be . . . F 0.11 0.04 29 + Cu 98.84 0.05 51 Sb < 11 + Na 0.110.01 30 + Zn < 52 Te < 12 Mg < 31 Ga <2e 0.003 53 I < 13 + Al 0.28 0.0232 Ge < 55 Cs <2e 0.003 14 + Si 0.58 0.03 33 As < 56 Ba 0.006 0.003 15 +P < 34 Se < Sum La . . . Lu 0.011 0.072 16 + S 0.0065 0.0006 35 Br <72 + Hf < 16 So 37 Rb < 73 + Ta < 17 + Cl 0.029 0.002 38 Sr < 74 W <18 + Ar 0.015 0.001 39 Y < 75 Re <2e 0.007 19 + K 0.0021 0.0007 40 Zr <76 Os <2e 0.007 20 + Ca 0.0041 0.0008 41 Nb < 77 + Ir 0.018 0.008 21 Sc< 42 + Mo <2e 0.002 78 Pt <2e 0.008 22 Ti <2e 0.001 44 Ru <2e 0.002 79Au < 23 V < 45 Rh < 80 Hg < 24 Cr < 46 Pd < 81 Tl < 25 Mn < 47 Ag <2e0.002 82 Pb < 26 Fe < 48 Cd <2e 0.002 83 Bi < 27 + Co < 49 In < 90 Th<2e 0.003 28 Ni < 50 Sn < 92 U < Light Elements Noble ElementsLanthanides 4 Be 44 Ru <2e 0.002 57 La <2e 0.005 5 B 45 Rh < 58 Ce < 6 C46 Pd < 59 Pr < 7 N 47 Ag <2e 0.002 60 Nd < 8 O 75 Re <2e 0.007 62 Sm <9 + F 0.11 0.04 76 Os <2e 0.007 63 Eu <2e 0.002 77 + Ir 0.018 0.008 64Gd < 78 Pt <2e 0.008 65 Tb <2e 0.002 79 Au < 66 Dy < 67 Ho < 68 Er < 69Tm <2e 0.004 70 Yb < 71 + Lu < KnownConc = 0 REST = 0 D/S = 0

[0438] TABLE 34 Quantum Catalytics, LLC ANALYSIS REPORT by UniquantOLD.613 of 7-Mar-02 Today 7-Mar-02 Spectrometers configuration: ARL 8410Rh 60 kV LiF220 LiF420 Ge111 TlAP Sample ident = 14-00-03 AX Furtherinfo = 14-00-03 AXIAL POLISHED VAC 3/7/02 Kappa list = 15-Nov-94 Channellist = 8-Jan-02 Calculated as: Elements Spectral impurity data: CAL.909Teflon (7/94) X-ray path = Vacuum Film type = No supporting film Casenumber = 0 Known Area, % Rest, Diluent/Sample and Mass/Area Eff. Diam. =25.00 mm Eff. Area = 490.6 mm2 KnownConc = 0% Rest = 0% Dil/Sample = 0Viewed Mass = 18000.00 mg Sample Height = 5 mm < means that theconcentration is < 20 ppm <2e means wt % < 2 StdErr. The + in Z + Elmeans involved in Sum = 100% Z wt % StdErr Z wt % StdErr Z wt % StdErrSum Be . . . F 0 0.043 29 + Cu 99.69 0.03 51 Sb < 11 + Na 0.039 0.01230 + Zn < 52 Te < 12 Mg < 31 Ga <2e 0.003 53 I < 13 + Al 0.103 0.008 32Ge <2e 0.002 55 Cs < 14 + Si 0.036 0.006 33 As < 56 Ba < 15 + P < 34 Se< Sum La . . . Lu 0.033 0.071 16 + S 0.0056 0.0005 35 Br < 72 + Hf < 16So 37 Rb < 73 + Ta < 17 + Cl 0.037 0.003 38 Sr < 74 W < 18 + Ar 0.0130.001 39 Y < 75 Re < 19 + K < 40 Zr < 76 Os < 20 + Ca 0.0048 0.0008 41Nb < 77 + Ir 0.031 0.008 21 Sc < 42 + Mo 0.005 0.002 78 Pt < 22 + Ti0.003 0.001 44 Ru < 79 Au <2e 0.007 23 V < 45 Rh < 80 Hg < 24 Cr < 46 Pd< 81 Tl < 25 Mn < 47 Ag < 82 Pb < 26 Fe < 48 Cd <2e 0.002 83 Bi < 27 +Co < 49 In < 90 Th < 28 Ni < 50 Sn < 92 U < Light Elements NobleElements Lanthanides 4 Be 44 Ru < 57 + La 0.015 0.005 5 B 45 Rh < 58 Ce< 6 C 46 Pd < 59 Pr < 7 N 47 Ag < 60 Nd < 8 O 75 Re < 62 Sm < 9 F < 76Os < 63 Eu <2e 0.002 77 + Ir 0.031 0.008 64 Gd < 78 Pt < 65 Tb < 79 Au<2e 0.007 66 Dy < 67 Ho < 68 + Er 0.015 0.004 69 Tm < 70 Yb < 71 + Lu <KnownConc = 0 REST = 0 D/S = 0

[0439] TABLE 35 Quantum Catalytics, LLC ANALYSIS REPORT by UniquantOLD.618 of 8-Jan-02 Today 7-Mar-02 Spectrometers configuration: ARL 8410Rh 60 kV LiF220 LiF420 Ge111 TlAP Sample ident = 14-00-03 RAD Furtherinfo = 14-00-03 RADIAL POLISHED VAC 3/7/02 Kappa list = 15-Nov-94Channel list = 8-Jan-02 Calculated as: Elements Spectral impurity data:CAL.909 Teflon (7/94) X-ray path = Vacuum Film type = No supporting filmCase number = 0 Known Area, % Rest, Diluent/Sample and Mass/Area Eff.Diam. = 25.00 mm Eff. Area = 490.6 mm2 KnownConc = 0% Rest = 0%Dil/Sample = 0 Viewed Mass = 18000.00 mg Sample Height = 5 mm < meansthat the concentration is < 20 ppm <2e means wt % < 2 StdErr. The + inZ + El means involved in Sum = 100% Z wt % StdErr Z wt % StdErr Z wt %StdErr Sum Be . . . F 0 0.042 29 + Cu 98.93 0.05 51 Sb < 11 + Na 0.230.02 30 + Zn < 52 Te < 12 Mg < 31 + Ga 0.008 0.003 53 I < 13 + Al 0.370.02 32 Ge <2e 0.003 55 Cs < 14 + Si 0.29 0.02 33 As < 56 Ba < 15 + P0.004 0.001 34 Se < Sum La . . . Lu 0.008 0.072 16 + S 0.021 0.002 35 Br< 72 + Hf < 16 So 37 Rb < 73 + Ta < 17 + Cl 0.068 0.006 38 Sr <2e 0.00174 W < 18 + Ar 0.018 0.002 39 Y < 75 Re < 19 + K 0.013 0.001 40 Zr < 76Os < 20 + Ca 0.017 0.002 41 Nb < 77 + Ir 0.023 0.008 21 + Sc 0.00360.0009 42 Mo < 78 Pt < 22 Ti < 44 Ru < 79 Au < 23 V < $$ Rh <2e 0.002 80Hg <2e 0.007 24 Cr < 46 Pd < 81 Tl <2e 0.005 25 Mn < 47 + Ag 0.004 0.00282 Pb <2e 0.003 26 Fe < 48 Cd <2e 0.002 83 Bi < 27 Co < 49 In < 90 Th <28 Ni < 50 Sn < 92 U < Light Elements Noble Elements Lanthanides 4 Be 44Ru < 57 La < 5 B 45 Rh <2e 0.002 58 Ce < 6 C 46 Pd < 59 Pr < 7 N 47 + Ag0.004 0.002 60 Nd < 8 O 75 Re < 62 Sm < 9 F < 76 Os < 63 Eu < 77 + Ir0.023 0.008 64 Gd < 78 Pt < 65 Tb <2e 0.002 79 Au < 66 Dy < 67 Ho < 68Er <2e 0.004 69 Tm < 70 Yb < 71 + Lu < KnownConc = 0 REST = 0 D/S = 0

[0440] TABLE 36 Quantum Catalytics, LLC ANALYSIS REPORT by UniquantOLD.612 of 7-Mar-02 Today 7-Mar-02 Spectrometers configuration: ARL 8410Rh 60 kV LiF220 LiF420 Ge111 TlAP Sample ident = 14-00-04 AX Furtherinfo = 14-00-04 AXIAL POLISHED VAC 3/7/02 Kappa list = 15-Nov-94 Channellist = 8-Jan-02 Calculated as: Elements Spectral impurity data: CAL.909Teflon (7/94) X-ray path = Vacuum Film type = No supporting film Casenumber = 0 Known Area, % Rest, Diluent/Sample and Mass/Area Eff. Diam. =25.00 mm Eff. Area = 490.6 mm2 KnownConc = 0% Rest = 0% Dil/Sample = 0Viewed Mass = 18000.00 mg Sample Height = 5 mm < means that theconcentration is < 20 ppm <2e means wt % < 2 StdErr. The + in Z + Elmeans involved in Sum = 100% Z wt % StdErr Z wt % StdErr Z wt % StdErrSum Be . . . F 0 0.042 29 + Cu 99.29 0.05 51 Sb < 11 + Na 0.070 0.01130 + Zn < 52 Te < 12 Mg < 31 Ga <2e 0.003 53 I < 13 + Al 0.27 0.02 32 Ge< 55 Cs <2e 0.003 14 + Si 0.29 0.02 33 As < 56 Ba <2e 0.003 15 + P < 34Se < Sum La . . . Lu 0.023 0.072 16 S 35 Br < 72 + Hf <2e 0.022 16 + So0.0074 0.0007 37 Rb < 73 + Ta < 17 + Cl 0.021 0.002 38 Sr < 74 W < 18 +Ar 0.012 0.001 39 Y < 75 Re < 19 + K 0.0023 0.0007 40 Zr < 76 Os < 20 Ca< 41 Nb < 77 + Ir 0.026 0.008 21 Sc < 42 Mo < 78 Pt <2e 0.007 22 + Ti<2e 0.001 44 Ru < 79 Au < 23 V < 45 Rh < 80 Hg <2e 0.006 24 Cr < 46 Pd <81 Tl < 25 Mn < 47 Ag < 82 Pb < 26 Fe < 48 Cd < 83 Bi < 27 Co < 49 In <90 Th < 28 Ni < 50 Sn < 92 U < Light Elements Noble Elements Lanthanides4 Be 44 Ru < 57 + La 0.013 0.005 5 B 45 Rh < 58 Ce < 6 C 46 Pd < 59 Pr <7 N 47 Ag < 60 Nd < 8 O 75 Re < 62 Sm < 9 F < 76 Os < 63 Eu < 77 + Ir0.026 0.008 64 Gd < 78 Pt <2e 0.007 65 Tb <2e 0.002 79 Au < 66 Dy < 67Ho < 68 Er <2e 0.004 69 Tm <2e 0.004 70 Yb < 71 + Lu < KnownConc = 0REST = 0 D/S = 0

[0441] TABLE 37 Quantum Catalytics, LLC ANALYSIS REPORT by UniquantOLD.619 of 8-Jan-02 Today 7-Mar-02 Spectrometers configuration: ARL 8410Rh 60 kV LiF220 LiF420 Ge111 TlAP Sample ident = 14-00-04 RAD Furtherinfo = 14-00-04 RADIAL POLISHED VAC 3/7/02 Kappa list = 15-Nov-94Channel list = 8-Jan-02 Calculated as: Elements Spectral impurity data:CAL.909 Teflon (7/94) X-ray path = Vacuum Film type = No supporting filmCase number = 0 Known Area, % Rest, Diluent/Sample and Mass/Area Eff.Diam. = 25.00 mm Eff. Area = 490.6 mm2 KnownConc = 0% Rest = 0%Dil/Sample = 0 Viewed Mass = 18000.00 mg Sample Height = 5 mm < meansthat the concentration is < 20 ppm <2e means wt % < 2 StdErr. The + inZ + El means involved in Sum = 100% Z wt % StdErr Z wt % StdErr Z wt %StdErr Sum Be . . . F 0 0.044 29 + Cu 98.59 0.06 51 Sb < 11 + Na 0.0620.012 30 + Zn < 52 Te < 12 Mg < 31 Ga <2e 0.003 53 I < 13 + Al 0.63 0.0332 Ge < 55 Cs < 14 + Si 0.60 0.03 33 As < 56 Ba < 15 + P < 34 Se < SumLa . . . Lu 0.021 0.073 16 + S 0.012 0.001 35 Br < 72 + Hf <2e 0.022 16So 37 Rb < 73 + Ta < 17 + Cl 0.020 0.002 38 Sr < 74 W < 18 + Ar 0.0160.002 39 Y < 75 Re <2e 0.009 19 + K < 40 + Zr 0.005 0.001 76 Os < 20 +Ca 0.0109 0.0010 41 Nb < 77 + Ir 0.035 0.009 21 Sc < 42 Mo < 78 Pt <22 + Ti 0.0037 0.0010 44 Ru <2e 0.002 79 Au < 23 V < 45 Rh < 80 Hg <2e0.006 24 + Cr 0.0020 0.0006 46 Pd < 81 Tl < 25 Mn < 47 Ag < 82 Pb < 26Fe < 48 Cd <2e 0.002 83 Bi < 27 Co < 49 In < 90 Th <2e 0.003 28 Ni < 50Sn < 92 U < Light Elements Noble Elements Lanthanides 4 Be 44 Ru <2e0.002 57 + La 0.010 0.004 5 B 45 Rh < 58 Ce < 6 C 46 Pd < 59 Pr 0.0050.002 7 N 47 Ag < 60 Nd < 8 O 75 Re <2e 0.009 62 Sm < 9 F < 76 Os < 63Eu < 77 + Ir 0.035 0.009 64 Gd <2e 0.002 78 Pt < 65 Tb <2e 0.002 79 Au <66 Dy < 67 Ho < 68 Er < 69 Tm < 70 Yb < 71 + Lu < KnownConc = 0 REST = 0D/S = 0

[0442] TABLE 38 Quantum Catalytics, LLC ANALYSIS REPORT by UniquantOLD.614 of 7-Mar-02 Today 7-Mar-02 Spectrometers configuration: ARL 8410Rh 60 kV LiF220 LiF420 Ge111 TlAP Sample ident = 15-00-01 AX Furtherinfo = 15-00-01 AXIAL POLISHED VAC 3/7/02 Kappa list = 15-Nov-94 Channellist = 8-Jan-02 Calculated as: Elements Spectral impurity data: CAL.909Teflon (7/94) X-ray path = Vacuum Film type = No supporting film Casenumber = 0 Known Area, % Rest, Diluent/Sample and Mass/Area Eff. Diam. =25.00 mm Eff. Area = 490.6 mm2 KnownConc = 0% Rest = 0% Dil/Sample = 0Viewed Mass = 18000.00 mg Sample Height = 5 mm < means that theconcentration is < 20 ppm <2e means wt % < 2 StdErr. The + in Z + Elmeans involved in Sum = 100% Z wt % StdErr Z wt % StdErr Z wt % StdErrSum Be . . . F 0 0.043 29 + Cu 99.21 0.04 51 Sb < 11 + Na 0.048 0.01230 + Zn < 52 Te < 12 Mg < 31 + Ga 0.008 0.003 53 I < 13 + Al 0.29 0.0232 Ge <2e 0.002 55 Cs <2e 0.003 14 + Si 0.37 0.02 33 As < 56 Ba < 15 + P< 34 Se < Sum La . . . Lu 0.011 0.072 16 + S 0.043 0.0004 35 Br < 72 +Hf <2e 0.022 16 So 37 Rb < 73 + Ta < 17 + Cl 0.021 0.002 38 Sr < 74 W <18 + Ar 0.014 0.001 39 Y < 75 Re <2e 0.008 19 + K < 40 Zr < 76 Os <2e0.007 20 Ca < 41 Nb < 77 + Ir 0.036 0.008 21 + Sc 0.0021 0.0009 42 Mo <78 Pt < 22 Ti < 44 Ru < 79 Au <2e 0.007 23 V < 45 Rh < 80 Hg < 24 Cr <46 Pd < 81 Tl < 25 Mn < 47 Ag < 82 Pb < 26 Fe < 48 Cd < 83 Bi < 27 Co <49 In < 90 Th < 28 Ni < 50 Sn < 92 U < Light Elements Noble ElementsLanthanides 4 Be 44 Ru < 57 La <2e 0.005 5 B 45 Rh < 58 Ce < 6 C 46 Pd <59 Pr < 7 N 47 Ag < 60 Nd < 8 O 75 Re <2e 0.008 62 Sm < 9 F < 76 Os <2e0.007 63 Eu < 77 + Ir 0.036 0.008 64 Gd < 78 Pt < 65 Tb < 79 Au <2e0.007 66 Dy < 67 Ho < 68 Er <2e 0.004 69 Tm < 70 Yb < 71 + Lu <KnownConc = 0 REST = 0 D/S = 0

[0443] TABLE 39 Quantum Catalytics, LLC ANALYSIS REPORT by UniquantOLD.617 of 8-Jan-02 Today 7-Mar-02 Spectrometers configuration: ARL 8410Rh 60 kV LiF220 LiF420 Ge111 TlAP Sample ident = 15-00-01 RAD Furtherinfo = 15-00-01 RADIAL POLISHED VAC 3/7/02 Kappa list = 15-Nov-94Channel list = 8-Jan-02 Calculated as: Elements Spectral impurity data:CAL.909 Teflon (7/94) X-ray path = Vacuum Film type = No supporting filmCase number = 0 Known Area, % Rest, Diluent/Sample and Mass/Area Eff.Diam. = 25.00 mm Eff. Area = 490.6 mm2 KnownConc = 0% Rest = 0%Dil/Sample = 0 Viewed Mass = 18000.00 mg Sample Height = 5 mm < meansthat the concentration is < 20 ppm <2e means wt % < 2 StdErr. The + inZ + El means involved in Sum = 100% Z wt % StdErr Z wt % StdErr Z wt %StdErr Sum Be . . . F 0 0.041 29 + Cu 99.39 0.05 51 Sb < 11 + Na 0.0930.012 30 + Zn < 52 Te < 12 Mg < 31 + Ga 0.007 0.003 53 I < 13 + Al 0.330.02 32 Ge <2e 0.002 55 Cs < 14 + Si 0.068 0.006 33 As < 56 Ba < 15 + P< 34 Se < Sum La . . . Lu 0.017 0.073 16 + S 0.0083 0.0007 35 Br < 72 +Hf < 16 So 37 Rb < 73 + Ta < 17 + Cl 0.034 0.003 38 Sr < 74 W < 18 + Ar0.017 0.002 39 Y < 75 Re < 19 + K 0.0053 0.0008 40 Zr < 76 Os < 20 + Ca0.0036 0.0008 41 Nb < 77 + Ir 0.031 0.008 21 Sc < 42 Mo <2e 0.002 78 Pt< 22 Ti < 44 Ru <2e 0.002 79 Au <2e 0.007 23 V < 45 Rh < 80 Hg <2e 0.00624 Cr < 46 Pd < 81 + Tl 0.014 0.005 25 Mn < 47 Ag < 82 Pb < 26 Fe < 48Cd < 83 Bi <2e 0.005 27 Co < 49 In < 90 Th < 28 Ni < 50 Sn < 92 U <Light Elements Noble Elements Lanthanides 4 Be 44 Ru <2e 0.002 57 La <2e0.005 5 B 45 Rh < 58 Ce < 6 C 46 Pd < 59 Pr < 7 N 47 Ag < 60 Nd < 8 O 75Re < 62 Sm < 9 F < 76 Os < 63 Eu <2e 0.002 77 + Ir 0.031 0.008 64 Gd <2e0.002 78 Pt < 65 Tb < 79 Au <2e 0.007 66 Dy < 67 Ho < 68 Er <2e 0.004 69Tm <2e 0.004 70 Yb < 71 + Lu < KnownConc = 0 REST = 0 D/S = 0

[0444] TABLE 40 Quantum Catalytics, LLC ANALYSIS REPORT by UniquantOLD.340 of 11-Jun-01 Today 11-Jun-01 Spectrometers configuration: ARL8410 Rh 60 kV LiF220 LiF420 Ge111 TlAP Sample ident = 15-01-03 AXIALFurther info = 15-01-03 AXIAL Fe, Cr, Mn, V 6/11 Kappa list = 15-Nov-94Channel list = 4-Jun-01 Calculated as: Elements Spectral impurity data:CAL.909 Teflon (7/94) X-ray path = Vacuum Film type = No supporting filmCase number = 0 Known Area, % Rest, Diluent/Sample and Mass/Area Eff.Diam. = 25.00 mm Eff. Area = 490.6 mm2 KnownConc = 0% Rest = 0%Dil/Sample = 0 Viewed Mass = 18000.00 mg Sample Height = 5 mm < meansthat the concentration is < 20 ppm <2e means wt % < 2 StdErr. The + inZ + El means involved in Sum = 100% Z wt % StdErr Z wt % StdErr Z wt %StdErr Sum Be . . . F 0 0.039 29 + Cu 0.028 0.002 51 Sb < 11 + Na 0.0320.009 30 + Zn 0.005 0.002 52 Te < 12 Mg < 31 Ga <2e 0.001 53 I <2e 0.00213 + Al 2.28 0.07 32 Ge < 55 Cs <2e 0.002 14 Si < 33 As < 56 + Ba <2e0.003 15 + P 0.0038 0.0003 34 Se < Sum La . . . Lu 0 0.21 16 S 35 Br <72 Hf <2e 0.004 16 + So 0.0092 0.0008 37 Rb < 73 Ta < 17 + Cl 0.0170.002 38 Sr < 74 W <2e 0.004 18 + Ar 0.009 0.001 39 Y < 75 Re < 19 + K <40 + Zr 0.045 0.004 76 Os < 20 + Ca 0.0060 0.0006 41 Nb < 77 Ir < 21 Sc< 42 Mo < 78 Pt < 22 Ti < 44 Ru < 79 Au < 23 + V 2.38 0.07 45 Rh < 80 Hg< 24 + Cr 2.71 0.08 46 Pd < 81 Tl < 25 + Mn 2.05 0.07 47 Ag < 82 Pb <26 + Fe 90.4 0.1 48 Cd < 83 Bi < 27 Co < 49 In < 90 + Th 0.005 0.00228 + Ni 0.012 0.003 50 Sn < 92 U < Light Elements Noble ElementsLanthanides 4 Be 44 Ru < 57 La < 5 B 45 Rh < 58 Ce < 6 C 46 Pd < 59 + Pr< 7 N 47 Ag < 60 Nd < 8 O 75 Re < 62 + Sm < 9 F < 76 Os < 63 + Eu < 77Ir < 64 Gd < 78 Pt < 65 + Tb < 79 Au < 66 Dy < 67 Ho < 68 + Er < 69 + Tm< 70 Yb < 71 Lu < KnownConc = 0 REST = 0 D/S = 0

[0445] TABLE 41 Quantum Catalytics, LLC ANALYSIS REPORT by UniquantOLD.339 of 4-Jun-01 Today 11-Jun-01 Spectrometers configuration: ARL8410 Rh 60 kV LiF220 LiF420 Ge111 TlAP Sample ident = 15-01-03 RADIALFurther info = 15-01-03 RADIAL Fe, Cr, Mn, V 6/11 Kappa list = 15-Nov-94Channel list = 4-Jun-01 Calculated as: Elements Spectral impurity data:CAL.909 Teflon (7/94) X-ray path = Vacuum Film type = No supporting filmCase number = 0 Known Area, % Rest, Diluent/Sample and Mass/Area Eff.Diam. = 25.00 mm Eff. Area = 490.6 mm2 KnownConc = 0% Rest = 0%Dil/Sample = 0 Viewed Mass = 18000.00 mg Sample Height = 5 mm < meansthat the concentration is < 20 ppm <2e means wt % < 2 StdErr. The + inZ + El means involved in Sum = 100% Z wt % StdErr Z wt % StdErr Z wt %StdErr Sum Be . . . F 0 0.036 29 + Cu 0.16 0.01 51 Sb < 11 + Na 0.0830.009 30 + Zn 0.032 0.003 52 Te < 12 + Mg 0.013 0.003 31 Ga <2e 0.001 53I < 13 + Al 4.5 0.1 32 Ge < 55 Cs < 14 + Si 0.15 0.01 33 As < 56 Ba <15 + P 0.0097 0.0009 34 Se < Sum La . . . Lu 0 0.20 16 S 35 Br < 72 + Hf0.018 0.004 16 + So 0.048 0.004 37 Rb < 73 Ta < 17 + Cl 0.032 0.003 38Sr < 74 + W 0.008 0.004 18 + Ar 0.010 0.001 39 Y < 75 Re < 19 + K 0.0190.002 40 + Zr 0.097 0.008 76 Os < 20 + Ca 0.051 0.004 41 Nb < 77 Ir <2e0.003 21 Sc < 42 Mo <2e 0.002 78 Pt < 22 + Ti 0.0030 0.0006 44 Ru < 79Au < 23 + V 2.26 0.07 45 Rh < 80 Hg < 24 + Cr 2.39 0.07 46 Pd < 81 Tl <25 + Mn 2.20 0.07 47 Ag <2e 0.001 82 Pb < 26 + Fe 87.9 0.2 48 Cd <2e0.001 83 Bi < 27 Co < 49 In < 90 + Th 0.006 0.002 28 Ni <2e 0.003 50 Sn< 92 U < Light Elements Noble Elements Lanthanides 4 Be 44 Ru < 57 La <5 B 45 Rh < 58 Ce < 6 C 46 Pd < 59 + Pr < 7 N 47 Ag <2e 0.001 60 Nd < 8O 75 Re < 62 + Sm < 9 F < 76 Os < 63 + Eu < 77 Ir <2e 0.003 64 Gd < 78Pt < 65 + Tb < 79 Au < 66 Dy < 67 Ho < 68 + Er < 69 + Tm < 70 Yb < 71 Lu< KnownConc = 0 REST = 0 D/S = 0

What is claimed is:
 1. A copper characterized by the x-ray fluorescencespectrometry plot of FIGS. 6A, 6B, 7, 25, or
 26. 2. A nickelcharacterized by the x-ray fluorescence spectrometry plot of FIGS. 27A,27B, 28A, 28B, 29, or
 30. 3. A cobalt characterized by the x-rayfluorescence spectrometry plot of FIGS. 31A, 31B, 32A, 32B, 33A, 33B, or34.
 4. A silicon characterized by the x-ray fluorescence spectrometryplot of FIGS. 45A, 45B, 46A, 46B, 47A, 47B, 48A, or 48B.
 5. An ironcharacterized by the x-ray fluorescence spectrometry plot of FIGS. 49A,49B, 50A, 50B, 51A, or 51B.
 6. A method of processing a metal or analloy of metals, comprising the steps of: (A.) adding the metal or alloyto a reactor in or more steps and melting said metal or alloy; (B.)adding a carbon source to the molten metal or alloy and dissolvingcarbon in said molten metal or alloy, followed by removing theundissolved carbon source; (C.) increasing the temperature of the moltenmetal or alloy; (D.) varying the temperature of the molten metal oralloy between two temperatures over one or more cycles; (E.) adding aflow of an inert gas through the molten metal or alloy; (F.) varying thetemperature of the molten metal or alloy between two temperatures overone or more cycles; (G.) adding a carbon source to the molten metal oralloy and dissolving carbon in said molten metal or alloy, followed byremoving the undissolved carbon source; (H.) varying the temperature ofthe molten metal or alloy between two temperatures over one or morecycles, wherein the molten metal or alloy has a greater degree ofsaturation with carbon than in Step (F.); (I.) stopping the flow of theinert gas; (J.) varying the temperature of the molten metal or alloybetween two temperatures over one or more cycles, wherein the moltenmetal or alloy has a greater degree of saturation with carbon than inStep (H.) and wherein an inert gas is added as the temperature islowered and an inert gas, chosen independently, is added as thetemperature is raised; (K.) varying the temperature of the molten metalor alloy between two temperatures over one or more cycles, wherein themolten metal or alloy has a greater degree of saturation with carbonthan in Step (J.) and wherein an inert gas is added as the temperatureis lowered and an inert gas, chosen independently, is added as thetemperature is raised; (L.) stopping the flow of the inert gases; (M.)varying the temperature of the molten metal or alloy between twotemperatures over one or more cycles, wherein the molten metal or alloyhas an equal or greater degree of saturation with carbon than in Step(K.); and (N.) cooling the molten metal or alloy to room temperature,thereby obtaining a solidified manufactured metal or alloy.
 7. A methodof processing a metal or an alloy of metals, comprising the steps of:(A.) adding the metal or alloy to a reactor in one or more steps andmelting said metal or alloy; (B.) adding a carbon source to the moltenmetal or alloy and dissolving carbon in said molten metal or alloy,followed by removing the undissolved carbon source; (C.) varying thetemperature of the molten metal or alloy between two temperatures overtwo or more cycles; (D.) adding a carbon source to the molten metal oralloy and further dissolving carbon in said molten metal or alloy,followed by removing the undissolved carbon source; (E.) varying thetemperature of the molten metal or alloy between two temperatures overtwo or more cycles, wherein the molten metal or alloy has a greaterdegree of saturation with carbon than in Step (D.); and (F.) cooling themolten metal or alloy to room temperature, thereby obtaining asolidified manufactured metal or alloy; further characterized by addinga flow of inert gas before, during, or after Steps (B.) through (E.). 8.The method of claim 6, wherein the metal is a transition metal.
 9. Themethod of claim 8, wherein the transition metal is chromium, manganese,iron, cobalt, nickel, copper, zinc, or alloys thereof.
 10. The method ofclaim 6, wherein the metal is an alkali metal or an alkaline earthmetal.
 11. The method of claim 6, wherein the metal is silicon.
 12. Themethod of claim 6, wherein the metal is aluminum.
 13. The method ofclaim 7, wherein the metal is a transition metal.
 14. The method ofclaim 13, wherein the transition metal is chromium, manganese, iron,cobalt, nickel, copper, zinc, or alloys thereof.
 15. The method of claim7, wherein the metal is an alkali metal or an alkaline earth metal. 16.The method of claim 7, wherein the metal is silicon.
 17. The method ofclaim 7, wherein the metal is aluminum.
 18. The method of claim 6,wherein the alloy of metals comprises copper, gold, and silver.
 19. Themethod of claim 6, wherein the alloy of metals comprises tin, zinc, andlead.
 20. The method of claim 6, wherein the alloy of metals comprisestin, sodium, magnesium, and potassium.
 21. The method of claim 6,wherein the alloy of metals comprises iron, vanadium, chromium, andmanganese.
 22. The method of claim 6, wherein the alloy of metalscomprises nickel, tantalum, hafnium, and tungsten.
 23. The method ofclaim 6, wherein the carbon source of Steps (B.) and (G.),independently, is a graphite rod, graphite powder, graphite flakes,diamond, fullerenes, natural gas, methane, ethane, propane, butane,pentane, cast iron, iron comprising carbon, or steel comprising carbon.24. The method of claim 6, wherein each cycle of Steps (D.), (F.), (H.),(J.), (K.), and (L.) comprises, in any order, a period of increasingmetal or alloy temperature and a period of decreasing metal or alloytemperature and wherein a cycle has a duration of 3 to 67 minutes. 25.The method of claim 24, wherein each cycle of Steps (D.), (F.), (H.),(J.), (K.), and (L.) comprises, in any order, a period of increasingmetal or alloy temperature and a period of decreasing metal or alloytemperature and wherein a cycle has a duration of 8 to 30 minutes. 26.The method of claim 6, wherein the period of increasing metal or alloytemperature in Steps (D.), (F.), (H.), (J.), (K.), and/or (L.),independently, is different than the period of decreasing metal or alloytemperature.
 27. The method of claim 6, wherein the period of increasingmetal or alloy temperature in Steps (D.), (F.), (H.), (J.), (K.), and/or(L.), independently, is equal to the period of decreasing metal or alloytemperature.
 28. The method of claim 6, wherein the inert gas of Steps(E.), (J.), and (K.), independently, is argon, nitrogen, helium, neon,xenon, hydrogen, krypton, and mixtures thereof.
 29. The method of claim6, wherein the molten metal or alloy of Step (N.) is cooled to roomtemperature by heat exchange with inert gas over 1 to 72 hours.
 30. Themethod of claim 6, wherein the molten metal or alloy of Step (N.) iscooled to room temperature by quenching in a bath comprising tap water,distilled water, deionized water, other forms of water, inert gases,liquid nitrogen or other suitable liquified gases, a thermally-stableoil or organic coolant, and combinations thereof.
 31. The method ofclaim 6, wherein the reactor is an induction furnace.
 32. A method ofprocessing copper, comprising the steps of: (A.) adding copper to areactor in one or more steps and melting copper; (B.) adding a carbonsource to the molten copper and dissolving carbon in the molten copper,followed by removing the undissolved carbon source; (C.) increasing thetemperature of the copper; (D.) varying the temperature of the moltencopper between two temperatures over 15 cycles; (E.) adding a flow of aninert gas through the molten copper; (F.) varying the temperature of themolten copper between two temperatures over 5 cycles; (G.) adding acarbon source to the molten copper and dissolving carbon in the moltencopper, followed by removing the undissolved carbon source; (H.) varyingthe temperature of the molten copper between two temperatures over 20cycles; (I.) stopping the flow of the inert gas; (J.) varying thetemperature of the molten copper between two temperatures over 4.5cycles, wherein an inert gas is added as the temperature is lowered andan inert gas, chosen independently, is added as the temperature israised; (K.) varying the temperature of the molten copper between twotemperatures over 15.5 cycles, wherein an inert gas is added as thetemperature is lowered and an inert gas, chosen independently, is addedas the temperature is raised; (L.) stopping the flow of the inert gases;(M.) varying the temperature of the molten copper between twotemperatures over 1 cycle; and (N.) cooling the molten copper to roomtemperature, thereby obtaining a solidified manufactured copper.
 33. Amethod of processing copper, comprising: (1.) contacting molten copperwith a carbon source; (2.) an iterative cycling process, whereinrelative saturation of copper with carbon remains the same or increasesindependently with each cycle; and (3.) cooling the molten copper toroom temperature, thereby obtaining a solidified manufactured copper.34. An alloy comprised of copper, gold, and silver characterized by thex-ray fluorescence spectrometry plot of FIGS. 35, 36, or
 37. 35. Analloy comprised of tin, lead, and zinc characterized by the x-rayfluorescence spectrometry plot of FIGS. 38, 39, or
 40. 36. An alloycomprised of tin, sodium, magnesium, and potassium characterized by thex-ray fluorescence spectrometry plot of FIGS. 41, 42, 43, or
 44. 37. Analloy comprised of iron, vanadium, chromium, and manganese characterizedby the x-ray fluorescence spectrometry plot of FIGS. 52, 53, 54, or 55.38. An alloy comprised of nickel, tantalum, hafnium, and tungstencharacterized by the x-ray fluorescence spectrometry plot of FIGS. 56,57, 58, 59, 60, or
 61. 39. A copper characterized by the x-rayfluorescence spectrometry plot of FIG.
 25. 40. A nickel characterized bythe x-ray fluorescence spectrometry plot of FIGS. 27A or 27B
 41. Acobalt characterized by the x-ray fluorescence spectrometry plot ofFIGS. 31A or 31B.
 42. A silicon characterized by the x-ray fluorescencespectrometry plot of FIGS. 45A or 45B.
 43. An iron characterized by thex-ray fluorescence spectrometry plot of FIGS. 49A or 49B.